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Pamantasan ng Lungsod ng Maynila

College of Engineering and Technology


Department of Chemical Engineering

THE PERFUME INDUSTRY

I. INTRODUCTION

Fragrance is a collective term, which refers to the manufacture of perfume,


cologne and toilet water. Its main purpose industrially is to produce a
pleasant scent for various products.

Perfume may be defined as any mixture of pleasantly odorous substances


incorporated in a suitable vehicle. Formerly, practically all products used in
perfumery were of natural origin. The finest modern perfumes are neither
wholly synthetic nor completely natural. The best product of the art is a
judicious blend of the two in order to enhance the natural perfume, to
reduce the price, and to introduce fragrances into the enchanting gamut
available.

II. BRIEF HISTORY


Fragrance has been existing for so long. Written accounts of its existence
dates back to the Egyptian times. It has also been mentioned in the Bible
numerous times. Fragrance was initially in the form of incense that was
discovered in Mesopotamia 4000 years ago. According to the book of
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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

Matthew, Chapter 2, the three Magi (or wise men) presented unto Jesus gifts
of gold, frankincense and myrrh. The process of extracting myrrh and
frankincense are identical, frankincense is a milky white resin extracted
from species of the genus Boswellia, which thrive in arid, cool areas of the
Arabian Peninsula, East Africa and India, while myrrh is a reddish resin that
comes from species of the genus Commiphora, which are native to northeast
Africa and the adjacent areas of the Arabian Peninsula. In 1100-1300 the
Crusaders brought home spices, bath ointments and essences that started a
new industry that flourished 200 years – the European perfume industry.
The Arab’s discovered distillation, the process of concentrating fragrant
essences. France flourished in the perfume industry during the 1500’s, they
used methods such as distillation, extraction and expression. Although the
birthplace of the first cologne was in Cologne, Germany its forerunner was
born in the 1600’s when a rosemary extract was mixed with a distilled
alcohol. The first Eau de Cologne was called 4711. From the 1970’s to the
present was the emergence of the different master perfumer’s, different
blends of fragrances and the development of methods in producing new
fragrances. Rene’ Coty created the Chypre wich is a blend of moss and
spices, Chanel #5 was made by Coco Chanel was considered as the first
modern perfume after the World War I. Other known perfumes were
Shalimar – an oriental blend by Guerlain, Vent Vert and L’Air du Temps.
Youth Dew, The Designer’s, The Blatants and the Sheers.

III. PERFUME INDUSTRIES IN THE PHILIPPINES

Green Cross, Inc, a manufacturing firm


specializing in health and hygiene and personal care
products, produces fragrance products like Lewis
and Pearl. The main office is located at 14th Floor
Common Goal Tower Finance corner Industry
Streets, Madrigal Business Park, Alabang,
Muntinlupa City Metro Manila, Philippines 1770.

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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

The Rogemson Company, Inc., situated


at 122 Old Samson Rd., Balintawak,
Quezon City, manufactures hair care,
personal, skin care, health and hygiene
products.

Avon Cosmetics, the leading fragrance-manufacturing firm in the


Philippines as of 2012 with a share of
43% of value sales and with
specializations in products like
perfumes, has its main office at 1139
Panorama Bldg., Brgy. Veterans Village,
Proj. 7, EDSA, Quezon City

IV. CONSTITUENTS OF PERFUME


Fragrance is not a single substance, it can be defined as a mixture of
pleasantly odorous substances incorporated in a suitable vehicles. The
words perfume, cologne, and air fresheners can fall under the fragrance
category. The difference between perfume and cologne is just their fragrance
concentration. Most perfume contains 30% fragrance while cologne contains
5% to a maximum of 8% fragrance. The components or the constituents of a
fragrance, or a perfume, are namely (1) VEHICLES, (2) FIXATIVES, and (3)
ODOROUS SUBSTANCES.

A. VEHICLES

Vehicles are modern solvents used for blending and holding the perfume
materials. It is mixed with more or less water according to the solubility of
oils employed and is volatile in nature. A good solvent should help to project
the scent it carries, should be fairly inert to the solutes, and is not too
irritating with the human skin.

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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

The perfect and most commonly used vehicle is the highly refined ethyl
alcohol. In perfume production, the slight natural odor of the alcohol is
removed by “deodorizing”. This is accomplished by adding small amount of
benzoin or other resinous fixatives to the alcohol and allowing it to mature
for a week or two. The result is an almost odorless alcohol.

B. FIXATIVES
 Fragrance Notes:

Top Notes – the scents that are perceived immediately on application of a


perfume. Top notes consist of small, light molecules that evaporate quickly.
They form a person's initial impression of a perfume.

Middle Notes - the scent of a perfume that emerges just prior to when the
top notes dissipate.

Base Notes - the scent of a perfume that appears close to the departure of
the middle notes. Base notes bring depth and solidity to a perfume and are
usually not perceived until 30 minutes after application.

A Perfume is made of volatile substances, and the more volatile


substances in it evaporate first. So, the series of top notes, middle notes, and
base notes will not be satisfied if the more volatile compounds which are
supposed to be in the base notes evaporate first. Thus, to solve this problem,
a fixative is added. We define fixative as substances of lower volatility than
the perfume oils, which retard and even the rate of evaporation of the
perfume constituents. There are three types of fixatives considered; the

1. Animal fixatives – come from the exudates or secretions of certain


animals.
2. Essential oil fixatives - essential oils that have a boiling point
higher than normal which ranges from 285 to 290 degree Celsius
3. Resinous Fixatives – these are normal or pathological exudates
from certain plants. There are hard resins, soft resins, moderately soft, and
oleoresins or oily materials.
4. Synthetic fixatives – synthetic fixatives are odorless esters. Some of
it are ethyl phthalate (295˚C), glyceryl diacetate (259˚C), and benzyl benzoate
(323˚C)

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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

C. ODOROUS SUBSTANCES

The odorous substances are the ones that give odor to a perfume. Under
odorous substances are (1) essential oils, (2) isolates, and (3) synthetic or
semi synthetic chemicals

(1) ESSENTIAL OILS

Essential oils can be defined as volatile, odoriferous oils that are obtained
from plant materials. Though both are of vegetable origin, essential oils differ
from vegetable oils in a way that they are volatile while vegetable oils are not.
Essential oils can be obtained from the leaves, flowers, fruits, seeds, barks,
and woods of a plant. Different essential oils can be obtained from different
part of the same plant. They are colorless to slightly yellowish when freshly
distilled, but the color may range from red to blue when foreign matter is
present, and becomes darker in color on the standing.

An Essential oil is not a single compound but a mixture of compounds


and some of the natural compounds occurring in it are:

Esters (e.ganethole, eucalyptole)


Alcohols (e.g. menthol, terpinol)
Aldehydes (e.g. benzaldehyde)
Phenols (e.g. eugenol, thymol)
Ketones (e.g camphor, menthone)
Lactones (e.g. coumarin)
Terpenes (e.g. camphene, pinene)
Hydrocarbons (e.g. cymene, styrene)

(2) ISOLATES

Isolates are pure compounds whose source is an essential oil or other


natural perfume material. Essential oil is a mixture of compounds, and when
a certain compound in an essential oil is derived or isolated; it is now called
an “Isolate”. Some notable examples are eugenol which is derived from clove
oil, santalol from sandalwood, and linalool from linaloa oil.

(3) SYNTHETIC AND SEMISYNTHETIC CHEMICALS

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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

Semisynthetic Chemicals are chemicals that are synthesized from isolate


or other natural starting materials. Examples are,

*Vanillin from eugenol from clove oil


*Ionone from citral from lemon grass oil

Synthetic Chemicals are substances that are chemically processed in the


laboratory and aren’t from natural occurring materials.

V. RAW MATERIALS

Chemical Structure

Vanillin

Glyoxylic Acid

Synthetic Vanillin
11,880 tonnes
Production
Natural Vanillin
120 tonnes
Production
Total Production 12,000 tonnes

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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

World production per year

The total annual production of vanillin is very small compared with a bulk
chemical like ammonia (130 million tonnes worldwide).

Although vanilla extract from pods is still used by the food industry, this
accounts for less than 1% of vanillin production. The remaining 99% is
obtained through synthetic routes. The lower cost of synthetic vanillin has
enabled its use as a chemical intermediate, and food use now accounts for
less than 50% of vanillin produced.

Vanillin is an organic compound with the molecular formula C8H8O3.


Natural vanillin is extracted from vanilla plant, Vanilla Planifola which
originated from the subtropicals of New Mexico and parts of Central America.
Freshly picked vanilla pods do not smell of vanilla, because the vanillin
molecule is immobilised by being bound to glucose. The smell of vanilla is
due to 200 different odorant molecules, but vanillin is the main one. It is
liberated when the pods are cured. Because of the scarcity and expense of
pure vanilla several methods of producing artificial vanilla has been
developed.

VI. REACTION

Most vanillin today are produced from the petrochemical raw material
guaiacol, there are several routes for synthesizing vanillin from guaiacol and
the most significant is two-step process is (1) guaiacol reacts with glyoxylic
acid by electrophilic aromatic substitution which results to a
vanillylmandelic acid (2) is then converted via 4-Hydroxy-3-
methoxyphenylglyoxylic acid (3) to vanillin (4) by oxidative decarboxylation.

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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

VII. PROCESS

A. MANUFACTURING PROCESS

1. Preliminary Treatment of Raw Materials

a. Alcohol Purification

Alcohol, which is used as a vehicle in perfume production, is first purified


through either alcohol alkali reflux or potassium permanganate oxidation.
The first involves the addition of sodium hydroxide in the raw alcohol. The
solution is then boiled for several hours and through one or more
fractionation, various fractions of vehicles of distinct aromas will be
collected. The latter involves the addition of potassium permanganate
solution in the alcohol and rapidly agitating the resulting solution after long
standing. Sediments are filtered out and the activated carbon is added. After
a few days, the remaining impurities in the solution are adsorbed in silica gel
filters to ensure purity. The purified alcohol is then subjected to aging at 15
degrees Celsius in a sealed vessel with small amount of flavors or spices for
one month.

b. Water Purification

Water is treated with EDTA or sodium citrate to ensure purity. The


resulting precipitate or complexes are removed through distillation or
sterilization.

2. Mixing or Blending

The pre-treated raw materials are placed and mixed in a perfume


manufacturing vessel made out of stainless steel or enamel, with silver or tin
lining in accordance to the proportions set. The mixture has to be stirred for
a while to hasten the precipitation of impurities from the flavors added. The
desired product must have improved clarity and anti-turbidity properties
under cold conditions.
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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

3. Aging

The manufactured perfume has to be stored in a storage vessel for aging.


Aging process has physical and chemical methods. Physical methods involve
air bubbling, mechanical agitation, infrared light exposure, ultraviolet light
exposure ultrasonic wave treatment or mechanical vibration. Chemical
methods, on the other hand involve oxygen or ozone bubbling, silver oxide or
silver chloride catalysis or tin or hydrogen reduction. The aging process of
perfumes involves the gradual ripening of the alcohol smell from being
rough. The length of time required to accomplish this process is dependent
on the conditions and other factors considered in the perfume production.

4. Chilling

The perfume subjected upon aging is now transported to the chilling


machine to be cooled. Perfume must be chilled in order to attain clarity and
to avoid translucency or turbidity under certain temperature changes.

5. Filtration

The insoluble materials are precipitated out and filtered in the filter press
to remove in order to ensure the clarity of the perfume. The perfume should
then be cooled at zero degrees Celsius and should be maintained at this
temperature while filtering. Filtration may cause the loss of some spices or
aroma and in advance, it has to be estimated and compensated afterwards.

6. Coloration

Coloration is done after the filtration operation to prevent the filtration of


the color or colors added. The resulting color of the product is needed to be
compared to that of the standard sample.

7. Quality Control or Product Testing

The quality and properties of the perfume are tested using certain
instruments to measure its refractive index, specific gravity, alcohol content,
etc.

8. Bottling

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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

If the perfume has passed the standards for product testing, it is now
ready for bottling. The bottles used are washed with distilled water and is
filled with perfume only up to the neck to prevent its breaking upon storage
due to thermal expansion.

9. Labeling and Packing

The perfume-filled bottles are now conveyed to the labeling station where
they are stamped. The labeled bottles are now transported to the packing
station to pack them in their containers. The packaging operation can be
done automatically, semi-automatically or manually.

B. EQUIPMENT

Alcohol Purifying Machine

The alcohol purifying machine is used to purify


the alcohol raw material. The picture in the left is a
silica gel filter which performs filtering procedure
by adsorbing the sediments or precipitates formed
in the alcohol upon its elution in the column.

Alcohol Storage Vessel

The filtered alcohol is treated with


spices and is aged and stored in a
flameproof alcohol storage vessel. Nitrogen
blanketing system of this vessel is

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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

dependent on the requirement of the plant


and is needed for minimal evaporation of the
vehicle.

Water Purifying Machine

Ideal water purifying equipment has


treatment schemes like carbon filter, sand
filter, micron filter and dozing.

Perfume Manufacturing vessel

The perfume raw materials are then transported


through piping lines with the aid of transport pumps to the
inlet of the perfume-manufacturing vessel. A paddle-type
impeller and shaft agitate the perfume mixture, which is
coupled with a flameproof motor mounted on top of the
vessel. The mixture is enclosed by a lid with gasket and
lock stud or knob to minimize the evaporation of the
alcohol.

Perfume Chilling Machine

The perfume from the manufacturing vessel is


transported through a pipeline by a transfer pump
to the inlet of the chiller. The perfume will then
pass through a number of plate heat exchangers
and after which, it is transported to a storage
vessel where its temperature is maintained at
temperatures approximately between -1 to -5 degrees Celsius. The insulation of
the vessel must be ideal for the preservation of the temperature of the perfume.
When the procedure is done, the perfume is settled down to the storage vessel
and is passed through the nitrogen gas in the plate heat exchangers to
preserve its scent.

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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

Filter Press

The filtering unit is flameproof and performs


filtering treatment through scavenger or
assembly plate and micron filter pad. The
output depends upon the viscosity, pH, nature
of the solid sediments or precipitates and the
contents of the liquid.

Perfume Filling Machine

The empty perfume bottle is taken and is placed on


the holders which are fixed to the rotary star wheel.
The rotary star wheel would keep on rotating and the
holders would push the bottle up towards the filling
head, the head would lock the bottle and due to
vacuum the filling would start, when the liquid is filled
up to the set level. The excess liquid would be
automatically sucked into the over-flow jar provided.
When the bottle comes down again, out from the filling
head, it is removed. The next batch of bottles will be
filled under the same procedure as the process goes on

PRODUCTION OF YLANG-YLANG (Cananga Odorata) ESSENTIAL OIL BY


FRACTIONAL STEAM DISTILLATION

I. Introduction

Ylang-ylang essential oil is one of the few essential oils extracted from
flowers that are exploited at a large scale. Ylang-ylang essential oil is distilled
from the mature fresh flowers of the Annonaceae family tropical tree Cananga
odorata [Lam.] Hook f. and Thomson forma genuina. The plant originates from

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College of Engineering and Technology
Department of Chemical Engineering

the Indonesian archipelago, but is currently exploited in the Western Indian


Ocean islands, mainly in Comoros Islands, Mayotte and Madagascar.

Ylang-ylang essential oil is mainly used by the cosmetic industry in


applications ranging from high grade perfume conception to soap manufacture,
but also, to a lesser extent, in aromatherapy or even as a food ingredient. In
addition to a great cultural and tourism value of the plant, the production of
ylang-ylang essential oil plays an important economic role as the oil represents
the second most important export product for the Comoros Islands, after
clovers.

II. History

1700s - French navigators searching for spices and new plants brought
back seeds of ylang-ylang to the French Territories of Mauritius in
the Indian Ocean. However the tree was regarded as a botanical
curiosity.

1800s - The economic potential of the tree was recognized and the
stimulation of the first phase of production with establishment of
vast plantation in Mauritius Islands.

1900s - On the initiative of the religious order of the “White Fathers”


in the island of Madagascar particularly on the Northwest and
Nosy-Be, the area was the source of ylang-ylang of the famous
“Peres Missionaires” brand.

- The first cultivation of ylang-ylang for commercial distillation was


established in the Philippines particularly on Northern Luzon
Island.

1910 - The increase in demand for ylang-ylang oil promoted the


establishment of new plantations on the Comoros Islands.

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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

At present, the production of Ylang-Ylang Essential Oil is a great


profit particularly in the areas of Central Luzon in the Philippines.
The demand for the bulk production of Ylang-ylang essential oil is
huge because Ylang-ylang essential oil is used for production of
cosmetics such as shampoo, liniments, etc.

III. Philippine Manufacturing Companies of Ylang-ylang Essential Oil

 ChemWorld Fragrance Factory


Ground Floor, Executive Building
Center, 369 Sen. Gil Puyat
Avenue cor. Makati Avenue, 1200,
Makati City

 Givaudan
Ortigas Center, Pasig City

 FM Group World
147 H. V. Dela Costa St. Salcedo
Village, Makati City

IV.Major Raw Materials

Raw Materials Structure Function

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College of Engineering and Technology
Department of Chemical Engineering

Ylang-Ylang Source of
Flower Essential Oil

Essential Oil
Water Carrier,
Condenser

V. Detailed Manufacturing Process

A. Preparation of Raw Material

 HARVESTING

The ylang-ylang tree flowers grow in bunches along the


branches and each has six petals which initially have a green
colour and then become yellow while maturing. The optimum
harvesting stage is when the centre of the ylang-ylang flower
displays a carmine crown.
The ylang-ylang flower is manually harvest and is carried out
early in the morning. Then the harvested flowers are then
collected and stored by the owners or distillers.

B. Conditioning of Raw Materials


 WATER PRE-HEATING

Before adding the ylang-ylang flowers, the water at the base


of the vessel is heated to boiling point.

C. Heart of the Process

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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

 FRACTIONAL STEAM DISTILLATION

Fractional Steam Distillation is the common method for


extracting aromatic compounds from lavender, eucalyptus,
particularly the ylang-ylang. Steam Distillation involves passing
steam through fresh plant material for over 18-24 hours, then
the ylang-ylang flower will reach over boiling point and some of
the aromatic compounds are altered by the exposure of heat.
The aromatic volatile oils from the ylang-ylang flower are
trapped with the steam and then cooled.

 CONDENSATION

Condensation process involves the transformation of the


steam into a liquid form. The liquid contains a mixture of water
and the ylang-ylang essential oil. In the condensation process,
the two separate and appear as a bottom layer of water and a
top layer of oils.

D. Refining

 OIL EXTRACTION

After the primary fractional steam distillation is completed


the ylang-ylang essential oil is collected. This primary extracted
essential oil is graded as “Extra”. The succeeding extracted oil
from the repeated use of the recent ylang-ylang flower will be
classified as “First” class, “Second” class and then “Third” class
for the last extraction of ylang-ylang essential oil.
 COOLING

After extracting the ylang-ylang oil, it is stored and cooled in


a storage tank for about 1 hour at a temperature of 27 degrees
Celsius.
 PACKAGING

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Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

After cooling the ylang-ylang oil, it is transferred in different


series of bottles with varying sizes and in bulk storage
containers and ready for shipment and export.

TABLE 1.1

Materials and Utilities Required to Produce 15 L of Ylang-Ylang Oil

Ylang-Ylang Flower 5-7kg

Water 70-80 L

Firewood 120 kg

Fuel 3.0-5.0 L

Direct Labor 21 working hours

Process Flow Chart

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College of Engineering and Technology
Department of Chemical Engineering

Figure 1: Process Flowchart of Ylang-Ylang Oil by Fractional Steam Distillation

Oil Grade Classification, Specification, and Yield

The grade classification for ylang-ylang oils has arisen through physic-
chemical criteria.

Grade Aroma Specific Refractive Index % of Total


Density (20°C) Distilled Oil
(20°C)

Extra Strong- 0.946-0.970 1.501-1.509 24%


floral

First Floral 0.933-0.945 1.500-1.510 10%

Second Duller 0.920-0.932 1.505-1.511 8%

Third Dull and 0.900-0.919 1.506-1.513 58%


Burnt

Chemical Composition of Ylang-Ylang Essential Oil

Chemical Structure % Composition

Linalool 48.6%

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College of Engineering and Technology
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Caryophyllene 10.7%

Germacrene 10.3%
Green D

p-Methylanisole 8.4%

Geranyl Acetate 7.6%

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College of Engineering and Technology
Department of Chemical Engineering

Benzyl Benzoate 7.6%

Benzyl Acetate 4.6%

Cadinene 4.6%

Humulene 2.8%

Benzyl 1.9%
Salicylate

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College of Engineering and Technology
Department of Chemical Engineering

Methyl 0.2%
Salicylate

1.1%

Cinnamyl
Acetate

V- Equipment for the Production of Ylang-Ylang Essential Oil

a) Feeding Tank

 The equipment used for loading


the water and the ylang-ylang
flower in fractional steam
distillation.

b) Distilling Condenser

 Distilling Condenser is used for


converting the steam containing
the ylang-ylang essential into
liquid form

c) Florentine Vase

 Florentine vase is the equipment


that separates the water and the
essential oil.

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College of Engineering and Technology
Department of Chemical Engineering

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College of Engineering and Technology
Department of Chemical Engineering

The Flavor Industry

Production of Chocolate Powder, Chocolate bar by Hot-pressing and


Conching

Definition of Chocolate

Chocolate is a typically sweet, usually brown, food preparation


of Theobroma cacao seeds, roasted and ground, often flavored, as with vanilla.
It is made in the form of a liquid, paste or in a block or used as a flavoring
ingredient in other sweet foods. Cacao has been cultivated by many cultures
for at least three millennia in Mexico and Central America. The earliest
evidence of use traces to the Mokaya, with evidence of chocolate beverages
dating back to 1900 BC. In fact, the majority of Mesoamerican people made
chocolate beverages, including the Mayans and Aztecs, who made it into a
beverage known as xocolātl, a Nahuatl word meaning "bitter water". The seeds
of the cacao tree have an intense bitter taste and must be fermented to develop
the flavor.
After fermentation, the beans are dried, cleaned, and roasted. The shell
is removed to produce cacao nibs, which are then ground to cocoa mass, pure
chocolate in rough form. Because the cocoa mass is usually liquefied before
being molded with or without other ingredients, it is called chocolate liquor.
The liquor also may be processed into two components: cocoa solids and cocoa
butter. Unsweetened baking chocolate (bitter chocolate) contains primarily
cocoa solids and cocoa butter in varying proportions. Much of the chocolate
consumed today is in the form of sweet chocolate, a combination of cocoa
solids, cocoa butter or other fat, and sugar. Milk chocolate is sweet chocolate
that additionally contains milk powder or condensed milk. White chocolate
contains cocoa butter, sugar, and milk but no cocoa solids.
Cocoa solids are one of the richest sources of flavanol antioxidants. They
also contain alkaloids such as theobromine, phenethylamine and caffeine.
These have physiological effects on the body and are linked to serotonin levels
in the brain. Some research has found that chocolate, eaten in moderation, can
lower blood pressure. The presence of theobromine renders chocolate toxic to
some animals, especially dogs and cats.
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College of Engineering and Technology
Department of Chemical Engineering

History of Chocolate

1500 BC: The Olmec Indians are believed to be the first to grow cocoa beans
(“kakawa”) as a domestic crop. Cacao trees have grown wild for possibly 10,000
years. The Olmec civilization lasts to about 300 B.C.

300 - 600 AD: The Aztecs cultivated the first cocoa plantations. The cocoa pod
symbolized fertility and life. Carvings from temple walls indicate cocoa pods
were often part of ceremonial and religious beliefs. They refer cocoa as being
the "god's food".

Cacao was used by the Maya as currency and in religious functions in addition
to its culinary applications. It was also the Maya who taught Europeans their
custom for drinking chocolate, though it is sometimes mistakenly attributed to
the Aztecs.

1492: Columbus brings back a few beans to present to the King and Queen.
However, they were mostly ignored amongst all the other wonderful array of
goods that were brought back.

1765: The first chocolate factory in America opens. The Baker Chocalate
Factory Dorchester Massachusetts

Dr. James Baker first began manufacturing chocolate on the banks of the
Neponset River in 1765. A Harvard-educated physician turned Dorchester
shopkeeper, Baker teamed up with John Hannon, an Irish immigrant, to
produce the dense, heavy chocolate "cakes" that early American colonists
ground by hand and mixed with boiling water to make a drinkable form of
chocolate, the popular way to enjoy it at the time.

1795: Steam engines are used to grind cocoa beans making chocolate cheaper

1847: The first chocolate bar is made by Joseph Fry & Son, chocolate
manufacturers, was founded by a Quaker who had been a doctor before
opening the business. The original Joseph Fry did not stick with chocolate, but
left the company to his sons so that he could become a typefounder. As the
successive generations of the family took over the business, they made steady
improvements. In 1789, his son (also named Joseph Fry) bought a Watts steam
engine to grind the cacao. In 1847, the firm under the leadership of the
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original Joseph Fry's great-grandson -- discovered a way to mix some of the


melted cacao butter back into defatted, or "Dutched," cocoa powder (along with
sugar) to create a paste that could be pressed into a mold. The resulting bar
was such a hit that people soon began to think of eating chocolate as much as
drinking it.

1849: Cadbury brothers are selling a similar product two years later. Joseph
Fry & Son and Cadbury Brothers display “chocolates for eating” at an
exhibition in Bingley Hall, Birmingham, England.

1875: Milk chocolate is invented. During the 1860s, the Swiss chocolate
manufacturer, Daniel Peter, tried repeatedly to create a chocolate bar flavoured
with milk, but he couldn't manage to produce a smooth mixture of milk and
chocolate. As it happened, in 1867, Henri Nestlé (also Swiss) was working on a
concentrated infant food formula, which required that he find a way to treat
milk so that it would not spoil while in storage but could be quickly
reconstituted for use. The result of his efforts, a sweetened condensed milk,
turned out to be perfect for Peter's purposes; the low water content made it
possible to mix it with the chocolate into a bar that did not spoil. By 1879,
Peter and Nestlé had joined to form a company. Nestlé has become the largest
food company in the world.

1908: Toblerone goes on sale. The Swiss chocolatier Jean Tobler, introduced
the triangular Toblerone bar.

Chocolate Companies in the Philippines

Delfi Foods Inc.

Delfi, an international Chocolate brand, bought Goya Philippines


sometime in 2011. Back then, we used to buy Goya products directly from this
plant at discounted prices. I’m not sure if they are still selling discounted
products at their plant.

Delfi (Goya) Factory is located at #23 M. Tuazon Street, Barangay Parang, here
in Marikina City.

It was in 1956, when the journey of the heritage brand began. The
families of Chua and Villabrille started to manufacture coffee and chocolates

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under the name of Philippine Cocoa. Throughout the years, this company has
been placed under the stewardship of different owners. In 1997, Philippine
Cocoa was acquired by Nestle.

Petra Foods—a publicly listed company in Singapore—came into the


picture in 2006 and they eventually bought Philippine Cocoa from Nestle.
Petra Foods is among the top three suppliers of cocoa in the world and it has
Delfi Corp. as its consumer marketing group.

As seen from above, the Goya bar varieties are: Raisins in Milk Chocolate, Dark
Chocolate, Raisins and Nuts in Milk Chocolate, Milk Chocolate, Cream White
Chocolate and Krispy Krunch: Milk Chocolate with Crisped Rice.

Annie Candy Manufacturing

Located at Jica Road, Buhay Na Tubig Imus, Cavite, Philippines

Known product is hany.

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Ricoa Philippines

COMMONWEALTH FOODS, INC. (Comfoods Inc.), a Filipino firm, is a


conglomeration of three pioneering food-manufacturing companies, which were
merged on September 30, 1968. The three corporations were: Commonwealth
Foods, Inc., Philippine Food Industries, Inc., and the Filipinas Biscuit
Corporation. With the merger, the three entities were reorganized into the Cofi
Division (for Roasted and Instant Coffee products), Philfood Division (for Cocoa
and Chocolate products), and Fibisco Division (for Biscuit products) of
COMFOODS. Located at Epifanio de los Santos Ave, Mandaluyong. Known
products are curly tops and flat tops.

Uses of Chocolates

Keeping Your Teeth Healthy

At first glance this might seem like an idea up there with chocolate

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teapots. After all, nobody’s dentist ever told them to eat more sweets. But it’s
true! According to researcher Arman Sadeghpour at Tulane University an
extract of cocoa powder found in chocolate could be an effective alternative to
using fluoride in toothpaste. In fact, if Sadeghpour’s research is correct, the
cocoa extract works even better than fluoride when it comes to fighting cavities.

As Legal Tender

Even more popular than “As useful as a chocolate teapot” is the


expression “Money doesn’t grow on trees!” Except that once upon a time it did.
The ancient civilisation believed to have first discovered chocolate, The Mayans,
actually used cocoa beans as money. It was a habit the Aztecs picked up as
well, even paying their taxes in cacao.

As Fuel

The chocolate powered car sounds like a dream, or a nightmare if you


don’t like the idea of having to share chocolate with your car. Scientists have
used surplus chocolate (we weren’t aware there was such a thing) to feed
Escherichia coli bacteria, who in turn produce hydrogen, which can be used as
a clean power source.

As A Weapon

As we covered recently, during World War II it was believed the Nazis


were going to try and assassinate Winston Churchill using a bomb disguised as
a bar of milk chocolate. The artist Lawrence Fish was called upon by the secret
service to illustrate that new, delicious looking threat. The idea was that when
you broke off chocolate from the end of the bar it would reveal “a piece of
canvas is revealed stuck into the middle of the piece” which, when pulled on,
would activate the bomb.

Fortunately such devices are no longer in use, so you can eat your
chocolate in safety.

Forms of Cocoa Beans Transformation

Cocoa Powder - Cocoa solids are a mixture of many substances remaining


after cocoa butter is extracted from cacao beans. When sold as an end product,
it may also be called cocoa powder, cocoa, and cacao. In contrast, the fatty
component of chocolate is cocoa butter. Cocoa butter is 50% to 57% of the

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weight of cocoa beans and gives chocolate its characteristic melting properties.
Cocoa liquor or cocoa mass is a paste of roasted cocoa beans with cocoa butter
and solids in their natural proportions. Chocolate requires the addition of extra
cocoa butter to cocoa liquor, and the excess cocoa solids resulting from the
chocolate industry dictate the relatively cheap supply of cocoa powder. This
contrasts with the earliest European usage of cocoa where, before chocolate
was popularized, cocoa powder was the primary product and cocoa butter was
little more than a waste product.

Cocoa Butter - Cocoa butter, also called theobroma oil, is a pale-yellow,


edible vegetable fat extracted from the cocoa bean. It is used to make
chocolate, as well as some ointments, toiletries, and pharmaceuticals. Cocoa
butter has a cocoa flavor and aroma.
Cocoa butter contains a high proportion of saturated fats, derived from
stearic and palmitic acids. Cocoa butter, unlike cocoa solids, has no more than
trace amounts of caffeine and theobromine.
Cocoa butter is obtained from whole cocoa beans, which are fermented,
roasted, and then separated from their hulls. About 54–58% of the residue is
cocoa butter. Chocolate liquor is pressed to separate the cocoa butter from the
cocoa solids. The Broma process is used to extract cocoa butter from ground
cacao beans. Cocoa butter is usually deodorized to remove its strong and
undesirable taste.

Chocolate – Mixture of cocoa powder, cocoa butter, sugar and other additives.

Major Raw Materials

Cocoa Bean

The cocoa bean, also cacao bean or simply cocoa or cacao, is the dried
and fully fermented fatty bean of Theobroma cacao, from which cocoa
solids and cocoa butter are extracted. They are the basis of chocolate, as well
as many Mesoamerican foods such as mole sauce and tejate.

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A cocoa pod (fruit) has a rough and leathery rind about 3 cm (1.2 in)
thick (this varies with the origin and variety of pod). It is filled with
sweet, mucilaginous pulp (called 'baba de cacao' in South America) enclosing
30 to 50 large seeds that are fairly soft and white to a pale lavender color.
While seeds are usually white, they become violet or reddish brown during the
drying process. The exception is rare varieties of white cacao, in which the
seeds remain white. Historically, white cacao was cultivated by the Rama
people of Nicaragua.
Cocoa is a deviation of the Spanish word cacao, derived from
the Nahuatl word cacahuatl. Cocoa can often also refer to the drink commonly
known as hot chocolate; to cocoa powder, the dry powder made by grinding
cocoa seeds and removing the cocoa butter from the dark, bitter cocoa solids;
or to a mixture of cocoa powder and cocoa butter.

Sugar
Sugar is the generalized name for sweet, short-chain, soluble
carbohydrates, many of which are used in food. They are carbohydrates,
composed of carbon, hydrogen, and oxygen. There are various types of sugar
derived from different sources. Simple sugars are called monosaccharides and
include glucose (also known as dextrose), fructose and galactose. The table or
granulated sugar most customarily used as food is sucrose, a disaccharide. (In
the body, sucrose hydrolyses into fructose and glucose.) Other disaccharides
include maltose and lactose. Longer chains of sugars are
called oligosaccharides. Chemically-different substances may also have a sweet
taste, but are not classified as sugars. Some are used as lower-calorie food
substitutes for sugar described as artificial sweeteners.

Sugar is a major ingredient of chocolate serves as preservative agent. For


effective preservation, the total sugar content should make up at least 65
percent of the weight of the final product. Sugar, which acts in much the same
way as salt, inhibits bacterial growth after the product has been heated. Sugar
comes from Hacienda Luisita in Tarlac of from Negros Occidental, Cebu and
Malaysia.

Additives

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Examples of additives that can be added in chocolate making include


microbial agents sodium benzoate, sorbic acid, calcium propionate; articial
sweetener (aspartame, saccharin); nutrient supplements (vitamins and
minerals); antioxidant, to prevent browning of fruits and other natural
processes ( vitamins E and C, BHA< BHT); flavour enhancers (salt, sugar,
monosodium glutamate); curing and pickling agents (nitrates and nitrites);
leavening agents (bromates, peroxides, ammonium chloride); stabilizers and
thickeners (gelatine, carrageenan, guar gum), and various approved color
additives.
Other additives that could make your chocolate better is adding milk,
nuts, etc.
Detailed Manufacturing Processes

Harvesting
Pods containing cocoa beans grow from the trunk and branches of the
cocoa tree. Harvesting involves removing ripe pods from the trees and opening
them to extract the wet beans.
Pods are suitable for harvest for 3 to 4 weeks, after which time the beans
begin to germinate. It is therefore necessary to harvest at regular intervals as
the pods do not all ripen at the same time. The frequency of harvesting can
have an effect on yield.
The pods are harvested manually by making a clean cut through the
stalk with a well sharpened blade. For pods high on the tree, a pruning hook
type of tool can be used with a handle on the end of a long pole. By pushing or
pulling according to the position of the fruit, the upper and lower blades of the
tool enable the stalk to be cut cleanly without damaging the branch which
bears it.
During harvesting it is important not to damage the flower cushion
which will produce the flowers and fruits of subsequent harvests, and care
must be taken not to damage the tree, which would make it easy for parasitic
fungi to penetrate the tissues of the tree.
Fermenting

Fermentation can be carried out in a variety of ways, but all methods depend
on removing the beans from the pods and piling them together or in a box to
allow micro-organisms to develop and initiate the fermentation of the pulp
surrounding the beans. The piles are covered by banana leaves.

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Fermenting of Cocoa Beans in a Wooden Crate

Yeast
Prominent yeast in the first 24 to 36 hours of fermentation include
Kloeckera apis (~70-90% of the total yeast grown), Kloeckera javanica and
Kloeckera africana, Candida pelliculosa and Candida humicola (less than 5% of
total yeast), Rhodotorula rubra and Rhodotorula glutinis. Saccharomyces
cerevisiae and Candida tropicalis were also prominent during first 24-36 hours,
but died off by the end of fermentation. Most grew only until about 37 to 40ºC,
and up to around 5-10% ethanol.

Lactic-Acid Bacteria
Lactic acid bacteria begin to grow when the pulp and “sweatings” are
degraded and drained, and the yeast are dying. The main function of lactic acid
bacteria is to metabolize pulp sugars (glucose and fructose) and citrate to
produce lactic acid, acetic acid, ethanol, and mannitol. The production of lactic
and acetic acid contributes to the decrease in pH. Lactic acid bacteria have also
been thought to contribute to yeast’s ability to use citrate as a carbon source.
These products are good for acetic acid bacteria growth, and allow them to
convert ethanol into acetic acid, releasing heat as a byproduct for the eventual
cocoa bean death.
Predominant lactic acid bacteria in the first 36 to 48 hours of
fermentation include Lactobacillus cellobiosus (60-85% of the total lactic acid
bacteria grown), Lactobacillus plantarum, Lactobacillus hilgardii (only 2% of
the total bacteria, Lactobacillus fermentum, Leuconostoc mesenteroides,
and Lactococcus lactis. Most grew well between 40 to 45ºC, and at 7 to around
10% ethanol.

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Acetic-Acid Bacteria
Towards the end of fermentation, the presence of yeast and lactic acid
bacteria decline and the fermenting heap becomes more aerated. These
conditions can therefore lead to the development of acetic-acid bacteria. This
bacteria oxidizes ethanol to acetic acid, and also further oxidizes the acetic acid
to carbon dioxide and water. These organisms are metabolized due to the
acidulation of cocoa beans at high temperatures, which causes diffusion and
hydrolysis of proteins in the cotyledons. Acetic acid bacteria primarily form the
precursors of chocolate flavor. These include members of the genus
Acetobacter as well as Gluconobacter.

Aerobic Spore-Forming Bacteria


High temperatures and increase in pH along with increased aeration
leads to the development of aeobic spore-forming bacteria of the
genus Bacillus. This includes B. pumilus, Bacillus licheniformis, Bacillus
subtilis, and Bacillus cereus. The Bacillus spp. found during the aerobic phase
of fermentation have been found to be responsible for the flavoring of chocolate.
Aerobic spore-forming bacteria form chemical compounds that cause acidity
and sometimes off-flavoring if fermentation continues for too long.

Filamentous Fungi
Filamentous fungi are also found in the well-aerated parts of the
fermented mass. They may cause hydrolysis of some of the pulp and produce
acids, but are not considered important in microbial succession. Of the
filamentous fungi, Aspergillus fumigatus and Mucor racemous are the most
present in the fungal population up to the end of fermentation. These fungi
cannot grow at temperatures higher than 45°C, but can be isolated at a
temperature of around 50°C.

Drying

When the beans are well fermented, they must be dried. Cocoa beans
may be dried in the sun. Spread the beans on boards raised 1 metre above
ground level. The layer of beans should not be very thick; not more than 4
centimetres. Stir the beans often and protect them from rain. To protect from
rain, you can make a little shelter and slide the boards under the shelter every
night and when it rains: This is called a sliding tray drier. Drying cocoa beans
takes five to ten days. In forest regions where the climate is very moist, cocoa
beans do not dry at all well. Badly dried beans are of poor quality. You get less
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money for them. In such regions several growers can get together and build a
modern drier. Spread the beans on a concrete slab set well above floor level.
Light a fire underneath, or allow hot air to pass through drums to heat the
concrete slab. Then the cocoa beans will dry better. In this way one man alone
can take care of drying the harvest of several growers. He should not let the fire
get too hot, to prevent the beans from becoming smoky. He should stir them
often so that they do not burn.

Cacao Beans dried in Tray Slides

Sorting

When the cocoa is quite dry, the beans are sorted. Remove all the flat
beans, germinated beans, mouldy beans, broken beans. Keep only good beans.
Put these good beans into sacks. Keep the sacks in a dry place well
protected against animals. Finally sell your sacks of cocoa Good-quality cocoa
is cocoa which has been well harvested, well fermented, well dried.

Roasting
After sorting all the beans by hand, it is next roaster. Each variety of
beans is roasted separately. Here is when the bean is heated 40.6 – 48.9°F,
which in turn, develops true chocolate flavour. It also reduces acidity and
astringency, lowers moisture content, deepens color and renders the kernel
more friable. As the beans rotate and dry inside the cylinder, their brown color
deepens, and their chocolate aroma intensifies.

Winnowing

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Following the roasting process, the beans are loaded into a machine
known as the winnower, which removes the hard outer hulls and separates the
‘nibs’ of the beans by size. The nibs are the basic product used for chocolate
production.

Milling

The part of the bean needed to make chocolate is the meat inside, called
the nib. To extract it, the newly roasted beans are quickly cooled, then sent
through a “cracker and fanner” that splits the thin brittle shells and blows
them away from the nibs. Mechanical sieves catch the broken pieces and sort
them by size.

Next, the nibs ride to the mills, where they are ground—in the same
process used since the time of the ancient Olmecs. Only now, the beans are
crushed mechanically between large grinding stones or heavy steel discs.
Modern mills produce so much pressure and friction that the cocoa butter, the
natural fat inside them, melts.

The newly liquefied beans are called chocolate liquor, but no alcohol is
involved. The term simply means "liquid." The liquor is poured into molds and,
when it hardens, is plain unsweetened chocolate.

If not destined to be sold as baking chocolate, this unsweetened


concoction is made into one of three different products, using two different
processes:

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Milling Machine

 Cocoa Powder and Cocoa Butter: By pressing it, to separate the two

 Eating Chocolate: By mixing it with extra cocoa butter, sugar and other
ingredients.

Alkalizing

Potassium bicarbonate is then added to neutralize the natural acids and


astringent and make cocoa easy to dissolve in liquid.

Dutch process chocolate or Dutched chocolate is chocolate that has been


treated with an alkalizing agent to modify its color and give it a milder taste
compared to "natural cocoa" extracted with the Broma process. It forms the
basis for much of modern chocolate, and is used in ice cream, hot cocoa, and
baking.
The Dutch process:

 Lowers acidity

 Increases solubility

 Enhances color

 Smooths flavor

Hot Pressing

To produce cocoa powder and cocoa butter, the unsweetened chocolate is


pumped into giant hydraulic presses that weigh up to 25 tons. Under pressure
—up to 6,000 pounds per square inch—the cocoa butter becomes a yellow
liquid that drains away through metallic screens and is collected for later use.
What remains is a dry, pressed brown cake that is cooled, pulverized, sifted
and sold as cocoa powder. Cocoa butter constitutes about half the weight of
the cocoa nib. This fat is partially removed from the cocoa liquor by means of

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hydraulic presses applying pressures as high as 450 kg/cm2. Depending upon


the pressing time and the setting of the press, the resulting cakes may have a
fat content of 10 to 24 percent. The cocoa liquor is subjected to pass the hot-
pressing pocess in order to remove predetermined amount of cocoa
butter/cocoa presscake.

Hydraulic Press

Pulverizing and Sifting

The cocoa presscake is then pulverized and sifted to produce cocoa


powder.

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Pulveriser

Cocoa powder use:

• Compound confectionery (25 %)

• Bakery and biscuit industry (25 %)

• Instant drinks production (25 %)

• Dairy and ice cream production (20%)

• Other, speciality uses (5 %)

Conching

The conching process redistributes into the fat phase the substances
from the dry cocoa that create flavor. Air flowing through the conche removes
some unwanted acetic, propionic, and butyric acids from the chocolate and
reduces moisture. A small amount of moisture greatly increases viscosity of the
finished chocolate, so machinery is cleaned with cocoa butter instead of
water. Some of the substances produced in roasting of cocoa beans
are oxidized in the conche, mellowing the flavor of the product.
The temperature of the conche is controlled and varies for different types
of chocolate. Generally higher temperature leads to a shorter required
processing time. Temperature varies from around 49 °C for milk chocolate to
up to 82 °C for dark chocolate. The elevated temperature leads to a

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partially caramelized flavor, and in milk chocolate promotes the Maillard


reaction.
The chocolate passes through three phases during conching. In the dry
phase, the material is in powdery form, and the mixing coats the particles with
fat. Air movement through the conche removes some moisture and volatile
substances, which may give an acidic note to the flavor. Moisture balance
affects the flavor and texture of the finished product because, after the
particles are coated with fat, moisture and volatile chemicals are less likely to
escape.
In the pasty phase, more of the particles are coated with the fats from
the cocoa. The power required to turn the conche shafts increases at this step.
The final liquid phase allows minor adjustment to the viscosity of the
finished product, which may be adjusted depending on the intended use of the
chocolate. Fats and emulsifiers are added to adjust the viscosity, and
thoroughly mixed.

Conche-Refiner
Standardizing (Tempering)

Cocoa butter is the fat in the cacao bean that gives chocolate its unique
mouth-feel and stable properties. To be considered “real” chocolate, a chocolate
bar or chunk can contain only cocoa butter, not any other fat. Cocoa butter is
the reason why you have to “temper” real chocolate.

Cocoa butter is fat that is composed of three to four glycerides of fatty


acids. What complicates matters in chocolate making is that each of these
different fatty acids solidifies at a different temperature. Once you melt a
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chocolate bar, the fatty acid crystals separate. The objective in tempering
melted chocolate is to entice the disparate fatty acid crystals of cocoa butter
back into one stable form.

Tempering is like organizing individual dancers at a party into a Conga


line. For chocolate, temperature and motion are the party organizers that bring
all the individual dancing crystals of fatty acids together in long lines and, in
the process, create a stable crystallization throughout the chocolate mass.

In the tempering process, melted chocolate is first cooled, causing the


fatty acid crystals to form nuclei around which the other fatty acids will
crystallize. Once the crystals connect, the temperature is then raised to keep
them from solidifying.

To help the chocolate to crystallize during the tempering process,


chocolate makers use one technique called seeding. The "seed" is tempered
chocolate in hunks, wafers or grated bits. It is added at the beginning of the
tempering process. These crystals of tempered chocolate act like magnets,
attracting the other loose crystals of fatty acids to begin the crystallization
process that results in well-tempered chocolate.

The final step before molding into bars and other shapes is tempering.
The cacao butter when cooled forms two kinds of crystals, stable and unstable.
Unstable crystals form gray streaks, known as bloom, in the final chocolate.
Also, the chocolate should have mostly stable crystals so it does not melt in the
hand. To remove the unstable crystals the chocolate is slowly heated to 118°F
(48°C) to melt all the fat crystals. Then it is cooled to 81°F (27°C) to set the
correct amount of stable fat crystals to provide the beginning of a structure
(seed crystals). Unfortunately, some unstable crystals are formed. To remove
these the chocolate's temperature is again increased to 90°F (32°C), which is
warm enough to melt the unstable crystals but not the stable crystals. In the
final molded chocolate the stable crystals give the bases to form the entire
chocolate with stable crystals.

Molding and Packaging

The final steps in the process are molding the chocolate, allowing it to
cool and harden, and then finally packaging it.

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Chocolate Molding Machine

Types of Chocolate

There are many kinds of chocolate available. Food regulations determine


whether a product can be called ‘chocolate’, generally requiring a minimum
of 20% cocoa solids and no more than 5% other fats. The ‘ingredients’
panel on the packaging will allow you to judge what type it is. Chocolate
should be kept in a cool, dry place, avoiding abrupt changes of temperature.
In suitable storage conditions and wrapped in foil it will keep for several
months. For maximum freshness purchase only when required.
There are four main types of chocolate for eating and cooking:

 Dark chocolate contains sugar, cocoa liquor or mass, cocoa butter and
flavourings. Couverture chocolate is a form of dark chocolate, generally
with more cocoa butter to give a good gloss and a ‘snap’ when broken
into pieces.
 Milk chocolate contains the same ingredients as dark chocolate, with at
least 20% chocolate liquor, and has milk solids added.
 White chocolate is a mixture of sugar, full-cream milk, cocoa butter and
flavourings
 Compound chocolate has all the ingredients of chocolate with added
vegetable fats, which help it to set at room temperature. It is the most
economical readily-available form of chocolate suitable for moulding at
school and does not need tempering. An example is NESTLÉ® Melts,
packaged in 375g waterproof packets in dark, milk, and white chocolate
varieties; available from supermarkets. There are also chocolate-like
materials for coating baked products. These contain a softer vegetable fat

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so a product can be cut without shattering the coating, but if it contains


more than 5% added fat it cannot be called chocolate.

Process Flowchart

FOOD ADDITIVES INDUSTRY

I. DEFINITION OF FOOD ADDITIVES

A food additive is any substance added to food that changes its


characteristics. Usually, it is a non-nutritive substance added deliberately to
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any food product in small amounts to improve its color, texture, taste, flavor,
consistency and shelf life. They integrate with the food item to become a
component, thereby improving its quality.

II. BRIEF HISTORY OF FOOD ADDITIVES

The use of food additives is not a modern-day invention. The practice


probably started when man first discovered that fire would cook and thereby
preserve his meat. Later he realized that the addition of salt would preserve
without cooking. In ancient times, cloves were placed in hams to inhibit the
growth of bacteria; the Egyptians used food colors and seasonings, spices,
flavors and condiments were considered so valuable as to serve as items of
trade and, at times, objects of war. The worth of spices during the Middle Ages
was measured in livestock and even, in some instances, in human lives. The
search for spices was the driving force behind many explorations including
those of Columbus who was seeking the spices of India when he discovered
America. As the United States moved from the late 1800’s into the 20th
century, sweeping changes took place throughout the country as Americans
moved from a rural environment to a more industrialized society. Advances in
farm mechanization and specialization, cross-country transportation systems,
the advent of canning, and later the development of refrigeration, all had an
impact on increasing this country’s food productivity to levels unheard of in
previous times. At the same time, America was demanding more from her food
supply, including increased availability and uniform quality. Industry
continues to satisfy consumer demands as we advance technologically. With an
everincreasing portion of our population employed in the working world, these
qualities take on further importance, as we require high-quality, readily
available foods.

III. TYPES OF FOOD ADDITIVES


1. Colouring

Food coloring is any dye, pigment or substance that imparts color when it is
added to food or drink. They come in many forms consisting of liquids,
powders, gels and pastes. Food coloring is used both in commercial food
production and in domestic cooking. Due to its safety and general availability,
food coloring is also used in a variety of non-food applications including
cosmetics, pharmaceuticals, home craft projects and medical devices.

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Purpose of Food Colouring

 Offset color loss due to exposure to light, air, temperature extremes,


moisture and storage conditions

 Correct natural variations in color

 Enhance colors that occur naturally

 Provide color to colorless and "fun" foods

 Make food more attractive and appetizing, and informative

 Allow consumers to identify products on sight, like candy flavors or


medicine dosages

Types of Food Colouring

a. Natural

Naturally occurring color additives from vegetable and mineral sources


were used to color foods, drugs, and cosmetics in ancient times. e.g. beta-
carotene, grape skin extract, caramel color, and saffron.

b. Synthetic

These man-made coloring agents are cheaper and more effective for
adding color compared to their natural counterparts that are derived from

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fruits, vegetables and minerals. e.g. FD&C Blue Nos. 1 and 2 and FD&C
Green No. 3

Types of certified color additives

a. Dyes dissolve in water and are usually used as powders, granules, or


liquids. They're commonly used in beverages, baked goods, confections
and dairy products.

b. Lakes do not dissolve in water, and are more stable than dyes, so they
are used for coloring food products contain fats and oils, or in products
that contain no moisture at all, such as cake mixes, hard candies and
chewing gum.

2. Preservative

Preservative is a substance that is added to products such as foods,


pharmaceuticals, paints, biological samples and wood to prevent
decomposition by microbial growth or by undesirable chemical changes. It is
usually used for protection against decay, discoloration, or spoilage.

IV. Classes of Preservative

Class I: Preservatives or the natural preservatives such as salt, sugar, vinegar,


syrup, spices, honey and edible oil.
Class II: Preservatives or the chemical preservatives such as benzoates,
sorbates, nitrites and nitrates of sodium or potassium, sulfites, glutamates and
glycerides.

Types of Preservatives

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a. Antimicrobials that destroy or delay the growth of bacteria, yeast and


molds. E.g. nitrites and nitrates prevent botulism in meat products.
Sulfur dioxide prevents further degradation in fruits, wine and beer.
Benzoates and sorbates are anti-fungal used in jams, salads, cheese and
pickles.

b. Anti-oxidants that slow or stop the breakdown of fats and oils in food
that happens in the presence of oxygen(Oxidation) leading to rancidity.
Examples of anti-oxidants include BHT, BHA, TBHQ, and propyl gallate.

c. Anti-enzymatic preservatives that block the enzymatic processes such


as ripening occurring in foodstuffs even after harvest. E.g. Erythorbic
acid and citric acid stop the action of enzyme phenolase that leads to a
brown color on the exposed surface of cut fruits or potato.

PRODUCTION OF TURMERIC OLEORESIN (Curcumin) BY DISTILLATION


WITH THE USE OF ACETONE

Introduction

Turmeric is an erect perennial plant grown as an annual crop for its


rhizome (underground rootlike stem bearing roots and shoots. The rhizome is
a deep bright yellow colour and similar form to the ginger but slightly smaller.
The plant originated in the Indian sub-continent and today India is the world’s
leading producer and consumer of turmeric. Turmeric plays an important role
in Indian culture- it is an essential ingredient of curry, used in religious
festivals, as a cosmetic, a cloth dye and in many traditional health remedies.
The spice is sometimes referred to as ‘Indian saffron’.

Turmeric is known as strengthening and warming to the whole


body. Traditional uses include to improve digestion, to improve intestinal
flora, to eliminate worms, to relieve gas, to cleanse and strengthen the liver and
gallbladder, to normalize menstruation, for relief of arthritis and swelling, as a
blood purifier, to warm and promote proper metabolism correcting both
excesses and deficiencies, for local application on sprains, burns, cuts, bruises,
insect bites and itches, for soothing action in cough and asthma, as
antibacterial and anti-fungus, and in any condition of weakness or debility.

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Another traditional use of turmeric is as a food colorant and dye for cloth – in
both cases a cheaper alternative to saffron.

I. History

1280 AD Marco Polo recorded information of


turmeric: “There is a vegetable which
contains all the properties of true saffron.
It also has the color and smell, yet it is not
actually saffron.”

1815 Scientist first isolated the curcumin


molecule.

1870 Scientist obtained the curcumin crystalline


form.

1910 Scientist determined curcumin’s overall


structure

II. Philippine Manufacturing Company of Turmeric Oleoresin

MSBIOGENESIS INTERNATIONAL CO.


Factory Location: Floridablanca, Pampanga
Address: Shaw Blvd., Mandaluyong, Metro Manila, Philippines

RAW MATERIALS

Raw Materials Structure Function

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Ethanol Used as Solvent

Contains essential oils


Turmeric(curcumin)

III. Detailed Manufacturing Process

A. Preparation of Raw Materials

Harvesting

Turmeric is harvested when the plants are between 7 and 10 months of age,
when the stems and leaves start to dry out and die back. The whole plant is
removed from the ground, taking care not to cut or bruise the rhizomes.

B. Conditioning of Raw Materials

Sweating

The leaves are removed from the plant and the roots carefully washed to
remove soil. Any leaf scales and long roots are trimmed off. The side (lateral)
branches (which are known as the fingers) of the rhizomes are removed from
the main central bulb (known as the mother). The mothers and fingers are
heaped separately, covered in

Drying

The rhizomes are sliced before drying to reduce the drying time and
improve the quality of the final product (it is easier to achieve a lower final
moisture content in small pieces of rhizome without spoiling the appearance of
the product). The rhizomes are traditionally sliced by hand, but there are small
machines available to carry out this process. The cooked fingers or bulbs are
dried until they have a final moisture content of 5-10%.
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Grinding

Grinding is a very simple process that involves cutting and crushing the
rhizomes into small particles, then sifting it through a series of screens of
different mesh size. There are a range of grinding mills available, both manual
and powered, of different capacities and which work in different ways. It can
be a method of adding value to a product. However, in general it is not
advisable to grind spices as they become more vulnerable to spoilage. The
flavour and aroma compounds are not stable and will quickly disappear from
ground products. The storage life of ground spices is much less than for the
whole spices.

C. Heart of the Process

Steam Distillation

Coarse-grinded turmeric is mixed with acetone in a stainless steel of


optimum dimensions. Direct steam is admitted from the bottom of the still. The
steam, which rises through the charge, carries along with it the vapors of the
volatile oils. By adding acetone or steam, the boiling points of the compounds
are depressed, allowing them to evaporate at lower temperatures, reducing the
deterioration of the desired products. Steam is passed through the plant
material containing the desired oils.

+  + ethanol

Ethanol(l) curcumin curcumin

Storage

Most essential oils can be stored for long periods under suitable conditions:
they should be dry, not in contact with the air or direct sunlight and kept cool.
It is important that essential oils do not come into contact with materials with
which they might react like rubber. Glass containers are often used for smaller
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amounts of oil but larger quantities are invariably stored in metal drums. Mild
steel drums lined with epoxy resin are very popular for essential oils. If
secondhand drums are to be used, it is important that they are thoroughly
cleaned and dried before being filled with essential oil. To ensure that the oil is
not wet it should be left to stand for some time before being filtered into its
container. Oils generally show no cloudiness when thoroughly dry. Freshly
distilled oils often possess some "still odours" which are unpleasant. These
generally disappear after several weeks storage

D. Refining

Drying

A composition having a curcuminoid and an essential oil of turmeric is


prepared by suspending the curcuminoid in water to form a suspension.
Essential oil is added to suspension to form a mixture; homogenizing the
mixture to obtain a fine slurry; and drying the fine slurry under heat and
vacuum.

Filtration

The fine slurry was extracted and filtered in preparation for the vacuum
distillation. Suspended solid matter is separated from a liquid, causing the
latter to pass through the pores of some substance.

Vacuum Distillation

All volatile solvents are evaporated off at ambient pressure. The


remaining liquid is allowed to cool down to room temperature. This way, the
low boiling components in the mixture evaporate away first. A variation of the
reduced-pressure process uses a vacuum pump to produce a very high
vacuum. This method is employed when dealing with substances that normally
boil at inconveniently high temperatures or that decompose when boiling under
atmospheric pressure.

Crystallization

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Curcumins are crystalized in purified form from the extract by


temperature induced solvent crystallization at a temperature in the range
between 5-30°C. The crystallized curcumin in pure form is separated from the
remaining liquid solution.

Storage and Packaging

Crystallized turmeric should be packaged in moisture proof, air-tight


polyethylene packages. It must be stored in a cool and dry environment, away
from direct sunlight. The bright colour of ground turmeric will fade when it is
left in the light for a long period of time. Therefore the packets should be stored
in a cardboard box, away from the sunlight.

PROCESS FLOWCHART

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Flavor Properties of Curcumin

Curcumin is an oil-soluble pigment, practically insoluble in water at


acidic and neutral pH, and soluble in alkali. In solutions the principal
colouring components of curcumin exhibit keto-enol tautomerism and,
depending on the solvent, up to 95 percent are in the enol form. The essential
oil fraction of the turmeric oleoresin has a very strong and bitter flavour, which
for many purposes, such as colouring of food products

Turmeric powder is obtained by dehydration and grinding of rhizomes.


Turmeric oleoresin, obtained by organic solvent extraction of turmeric, is a
brownish-orange viscous oily product containing 30 to 55% curcuminoid
pigments and 15 to 25% volatile oil. Both turmeric powder and oleoresin can
only be used in food products in which the flavor characteristic of turmeric is
desirable, e.g. pickles, mustard, mayonnaise, frozen fish fillet coating, meat

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products and pastries (Abea, 1984). Curcumin is the colorant without residual
turmeric flavor.

The solubility of curcumin in some organic solvents is: acetone > ethyl
methyl ketone > ethyl acetate > methanol > ethanol > 1 ,2 dichloroethane >
isopropanol > ether > benzene > hexane.

PRODUCTION OF MONOSODIUM GLUTAMATE BY GLUTAMIC ACID


FERMENTATION
(Sugar Cane Molasses as a Source of Glucose)

Introduction

Glutamic acid is an amino acid that is one of the important components


of protein that our bodies need. It is referred to as “non-essential” amino acid
because humans do not need to eat glutamic acid or eat protein that contains
glutamic acid in order to supply the body with the glutamic acid that it needs.
Glutamic acid can be produced via fermentation of glucose through glutamic
acid producing bacteria. Widely used source of glucose are sugar cane
molasses.

Monosodium glutamate (MSG) is a sodium salt of the glutamic acid.


Large quantities of monosodium glutamate have been used as a flavour
intensifier. It is claimed by some authors that this compound has little or no
flavour itself but intensifies the flavour of meats and vegetables through a
rounding or blending effect.

Reports that the use of MSG in foods is harmful were denied by a


National Academy of Science – National Research Council report in 1971. In
1974, the Food and Agricultural Organization of the World Health Organization
approved the use of MSG as safe.

IV. History

1886 - German Chemist Ritthausen isolated glutamic acid as


a pure substance through acidic hydrolysis of gliadin,
a component of wheat gluten.

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1908 - Japanese Chemist Kikunae Ikeda found that glutamic


acid was responsible for the flavour enhancing
properties of the kelp-like seeweed, “konbu,” that had
been used for many centuries in Japan in the
preparation of soup stocks.

1909 - The first monosodium glutamate was produced


commercially under the trade name Ajinomoto.

1956 - Shikuo Kinoshita discovered an industrial processing


technique, which allowed commercial scale production
of MSG from mass fermentation, and was granted a
15-year patent.

At present, Ajinomoto Company is the world’s largest producer of


MSG holding a 35 to 40% share of the world market.

V. Philippine Manufacturing Company of MSG

 331 Sen. Gil Puyat Ave.


MakatiCity, NCR - Fourth
District 1200

 Philippines largest
producer of MSG

VI. Major Raw Materials

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Raw Materials Structure Function

Sugar Cane source of carbohydrates


Molasses

glutamate producing
coryneform bacteria
bacteria

source of nitrogen; maintain


Urea ( Ammonia ) the pH of the culture

Sodium Hydroxide neutralizer


(NaOH)

Hydrochloric Acid acidifier; convert the


(HCl) residual carbohydrates into
humin

VII. Detailed Manufacturing Process


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A. Preparation of Raw Material

 HARVESTING

The sugar cane is harvested


through sugar cane harvester.
Essentially a storage vessel on a
truck with a mechanical
extension, the machine cuts the
stalks at the base, strips the
leaves off, and then cuts the
cane into segments. These are
then deposited into either the
on-board container, or a
SUGAR CANE HARVESTER separate vehicle traveling
alongside. Waste material is then ejected back onto the field,
where it acts as fertilizer

 EXTRACTION OF MOLASSES

The sugar canes are


juiced with the use of
sugar cane top table
crusher.

SUGAR CANE TOP TABLE


B. Conditioning of Raw Materials CRUSHER

 MICROBIAL FERMENTATION OF GLUTAMIC ACID

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Reaction:

C12H22O11 +
3O2 + 2NH3

2C5H9O4N + 2CO2 + 5H20

FERMENTING TANK

In fermentation, Glutamic Acid is synthesized by coryneform bacteria,


specifically Corynebacterium glumamicum, Brevibacterium lactofermentum, and
Brevibacterium flavum. These glutamate-producing bacteria are gram positive,
non-spore-forming, and nonmotile, and required biotin for growth. But when
biotin is present in sufficient concentration for an optimal rate of proliferation,
only inferior amount of glutamate is accumulated because the cell membrane
is impermeable to it. But cane molasses (source of glucose) in which the
bacteria is usually cultured are rich in biotin, that is why biotin-inhibiting
additives are added such as penicillin. In this way, the ultimate concentration
of glutamic acid could be achieved without biotin limitation. Moreover,
necessary nitrogen could be supplied by ammonium salts, and urea, or best
by gaseous ammonia, which could not only provide the nitrogen but also
maintain the pH of the culture medium between 7 and 8 without diluting the
culture medium. And since the fermentation is aerobic, oxygen is provided by
passing compressed air into the fermenting mixture , and the fermenter is
stirred. The optimum temperature for fermentation is 30 degrees celcius.
Fermentation is an exothermic reaction and the temperature critically affects
the not only the propagation of microorganisms, but also the formation of
glutamic acid. The medium and all materials are sterilized, and all operations
and variables, including temperature, pH, and dissolved oxygen concentration,
are automatically controlled during the 35-45 hour time for fermentation.

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 CENTRIFUGATION

At the end of the fermentation, the


fermented broth is sterilized, and
then supercentrifuged to remove the
used microorganisms and any other
solid or impurities by the clarifier
centrifuge. The mixture to be clarified
enters the rotor through a centrally
arranged feed tube. The distributor
accelerates the product and conveys
it into the separating space to the

CLARIFIER CENTRIFUGE
disc stack where the actual separation of
solids and liquid takes place. The configuration of the bowl takes into
consideration the flow characteristics (fluidics). The flow behaviour of the solids
is particularly important. Because of their higher density, they are flung
against the underside of the disc above and flow down into the disc stack.

 EVAPORATION

The evaporator is where the dilute


solution consisting of a non-volatile
solute which is the glutamic acid,
and volatile solvent (water) being
concentrated to a thick liquor of
glutamic acid. In this stage, the
stream is used in heating the
solution.

EVAPORATOR

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 HYDROLYSIS

Reaction:
C5H9O4N+ HCl
C5H9O4N.HCl

HYDROLYZER

The thick liquor or slurry produced from is then fed to the hydrolyzer which is
lined glass, adding in to the slurry a 30% hydrochloric acid. The glutamic acid
fermentation broth is almost neutral and the glutamic acid is usually present
as mono-sodium or Amono-ammonium glutamate. In order to make such a
broth strongly acid, it is necessary to add inorganic acid in an amount
equivalent to sodium or ammonium of the glutamates, and further to combine
with glutamic acid to form the inorganic acid salt of glutamic acid, for example
glutamic acid hydrochloride or hydrosulfate, and furthermore to hydrolyze the
cells and convert the residual carbohydrates to humins.

 NEUTRALIZATION

Reaction:

C5H10O4NCl +
NaOH

C5H9O4N + NaCl
+ H2O

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NEUTRALIZER

After the hydrolysis reaction is completed, the solution goes to the neutralizer
where a sodium hydroxide solution, or any other sodium base, is used as a
neutralizing agent for the excess hydrochloric acid that is not reacted in the
hydrolyzer. Here, the pH is adjusted to the isoelectric pH which is 3.22.
Isoelectric pH is the pH of minimum solubility where the average charge is
zero. The average charge is zero at this pH because most of the time the
glutamic acid molecule is present as 2 (charge=), half of the rest of the time as
1 (charge= +1), and half of the rest of the time as 3(charge=-1). The isoelectric
pH of 3.22 is exactly halfway between 2.19 and 4.25. (See figure 1) If the pH is
above 3.22, acid is converted to a very soluble sodium salts, and if the pH is
below, the acid dissolves in water. The neutralizer is made up of lead-lined
steel tanks to guard against the etching action of the caustic soda. The reaction
proceeds at room temperature and conditions, 30 degree Celcius and 1 atm.

Figure 1: Isoelectric point of Glutamic Acid

 GLUTAMIC ACID CRYSTALLIZATION

From the neutralizer, the resulting


product goes to the glutamic acid
crystallizer where the crystals of glutamic
acid are formed. Here, the solution is

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cooled to 65-75 degrees farenheit. During the cooling, the glutamic acid
precipitated in large pure crystals.

CRYSTALIZING TANK
 FILTRATION BY DECANTER
CENTRIFUGE

The glutamic acid crystals formed in


the glutamic acid crystallizer are now
separated in the superdecanter
centrifuge. The mother liquor goes out
of the first filtration. This mother
liquor, upon pH adjustment by the
ammonia, can be used as a liquid
fertilizer.

DECANTER CENTRIFUGE

C. Heart of the Process

 DISSOLUTION

Reaction:

C5H9O4N +
NaOH

C5H8NO4Na+
H2O

NEUTRALIZER
The crystals are then introduced to the dissolver where the caustic soda
solution is added. In this stage, the neutralization takes place between the
caustic soda solution and the crystals of glutamic acid. Thus, producing crude

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to its brownish color that might be caused by the raw materials and
microorganisms employed during fermentation.

D. Refining

 DECOLORIZATION

From the dissolver, the crude


solution is transported to a
decolorizer whereby activated
carbon is used. Active carbon has
many microholes on its surface.
Impurities are adsorbed onto the
surface of active carbon.
Monosodium glutamate solution
becomes clean and clear.
DECOLORIZER

 MSG CRYSTALLIZATION

The clear solution obtained is transferred to the MSG crystallizer to form MSG
crystals. The solution containing MSG is heated to supersaturation or
evaporation.

 DRYING
 DRYING

The MSG crystals proceed to the dryer


to reduce the moisture content but
not completely removed. Drying is
carried out at 90 degrees celcius.

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DRYER

 SCREENING

After drying, the crystals are screened for the purpose of classification. Fine,
medium, and large crystals are sorted out.

 PACKAGING

Later on, the classified crystals are


brought to the packaging section ready
for shipment.

PACKAGING MACHINE
Materials and Utilities Required to Produce 1 ton of MSG.H 2O

Sugar 1.5 – 2.5 ton

Electricity 79, 200 MJ

Fuel 46.6 MJ

Direct Labor 17.6 work-h

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Process Flow Chart

Figure 2: Process Flowchart of Monosodium Glutamate Production by Fermentation

Flavor Properties of Monosodium Glutamate Produced

The taste threshold for monosodium glutamate is about 0.3 grams in a


liter of water, considerably lower than the taste thresholds for salt (2 g/L) or
sugar (sucrose; 5 g/L). The flavor sensation of MSG is unlike that of any of the
other four or five basic flavor sensations of sweet (sucrose), sour (lemon juice),
salt (sodium chloride), bitter (quinine), or pungent (mustard or chili peppers).
The flavor sensation of MSG is often described as “meaty” and has been given
the name “umami” (deliciousness). In addition, MSG has the ability to enhance
natural taste.

MSG also has a strong synergistic effect with disodium inosinate and
disodium guanylate, which are found in meat, fish, vegetables, and
mushrooms. These substances are almost tasteless in the absence of MSG, but
addition of even a small quantity of MSG to food that contains these
nucleotides produces an umami that is as much as six or eight fold greater
than that to be expected from the quantity of MSG added.

Fragrance, Flavors and food Additives 163

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