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PROCESS OPTIMIZATION OF SPRAY DRYING OF

BEETROOT JUICE
Thesis submitted in partial fulfilment
For the award of the degree of

BACHELOR OF TECHNOLOGY
In

AGRICULTURAL ENGINEERING
By

PRITHA ROY
Roll 082117 No. 31330366
SWARMISTA PAUL
Roll 082117 No. 31330377

Under the supervision of

ER. GAJENDRA PRASAD

DEPARTMENT OF AGRICULTURAL ENGINEERING


TRIGUNA SEN SCHOOL OF TECHNOLOGY
ASSAM UNIVERSITY (A CENTRAL
UNIVERSITY) SILCHAR- 788 011, ASSAM
AUGUST, 2021
DEPARTMENT OF AGRICULTURAL ENGINEERING
TRIGUNA SEN SCHOOL OF TECHNOLOGY
ASSAM UNIVERSITY (A CENTRAL UNIVERSITY)
SILCHAR – 788 011, ASSAM

CERTIFICATE OF APPROVAL
This is certify that the thesis entitled “Process Optimization of Spray Drying of Beetroot Juice”
submitted by Pritha Roy & Swarmista Paul, student of Department of Agricultural
Engineering, during the year 2017-2021 to Assam University, Silchar, for the award of Bachelor
of Technology has been accepted by the external examiner and that the students have
successfully defended the thesis in their viva – voce examination held today.

(Supervisor) (External Examiner) (Head of Department)

(Seal of the Department)

i
DEPARTMENT OF AGRICULTURAL ENGINEERING
TRIGUNA SEN SCHOOL OF TECHNOLOGY
SILCHAR – 788 011, ASSAM
ASSAM UNIVERSITY (A CENTRAL UNIVERSITY)

CERTIFICATE OF SUPERVISORS

Certified that the thesis entitled “Process Optimization of Spray Drying of Beetroot Juice”
submitted by Pritha Roy & Swarmista Paul at Assam University, Silchar, is a record of
bonafide project work under my supervision and is worthy of consideration for the award of the
degree of Bachelorof Technology of the Institute.

Date: 11/8/2021 (Er. Gajendra Prasad)


Place: Silchar Supervisor

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ACKNOWLEDGEMENT

We express our deep sense of gratitude to our supervisor Er. Gajendra Prasad,
Assistant Professor of Department of Agricultural Engineering, Assam University, Silchar for his
constant encouragement, invaluable guidance and all possible help that have enabled us to bring
this research work to a successful completion.

We immensely indebted to Dr. Laxmi Narayan Sethi, Dean, TrigunaSen School of


Technology, Assam University, for providing the necessary facilities during the course of study.

We also express my sincere gratitude and indebtedness to Dr. Laxmi Narayan


Sethi, Dr. Ajita Tiwari, Dr. Chetan Khobragade, Dr. Avinash Kumar, Mr. Ghanshyam Gogoi,
Er. Swastika Das, Er. M. Padhiyary, Er. Anamika Yadav and our staffs for their help and
encouragement in successful completion of the thesis.

We are grateful to the Hon’ble Vice Chancellor, Assam University, Silchar, Prof.
Dilip Chandra Nath, for providing us the much needed facilities.

We owe a lot to our parents for their blessings and love who have shouldered
innumerable difficulties enabling us to achieve our goal. We think simple dedicatioin of this tiny
piece of research work would not be sufficient to repay their perpetual work unconditional
support.

Date: 11/08/2021

Place: Silchar (Pritha Roy) (Swarmista Paul)

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DECLARATION

We hereby declare that the project entitled “Process Optimization of Spray Drying of
Beetroot Juice” submitted for the Degree of Bachelor of Technology of the Department of
Agricultural Engineering, during the year 2017-2021 to Assam University, Silchar is our original
work and the dissertation has not formed the basis for the award for any degree, associate ship,
fellowship or any other similar title.

Date: 11/08/2021

Place: Silchar (Pritha Roy) (Swarmista Paul)

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TABLE OF CONTENTS

Title Descriptions Page No.

TITLE PAGE i

CERTIFICATE OF APPROVAL ii

CERTIFICATE OF SUPERVISORS iii

ACKNOWLEDGEMENTT iv

DECLARATION v

TABLE OF CONTENTS vi

LIST OF TABLES X

LIST OF FIGURES xii

LIST OF ABBREVIATIONS xiv

LIST OF NOTATION xvi

ABSTRACT xvii

CHAPTER I INTRODUCTION 1-4

1.1 Background 1

1.2 Objectives 4

CHAPTER II REVIEW OF LITERATURE 5-12

2.1 General 5

2.1.1 Spray Dryer 5

v
2.1.2 Basic Considerations 7

2.1.2.1 Spray Drying Steps 7

2.1.2.2 Operating Conditions 8

2.1.2.3 Powder Properties 8

2.1.2.4 Stickiness during Spray Drying 8

2.1.2.5 Methods of Spray Drying Sugar rich Foods 9

2.1.2.6 Addition of Drying Aids 10

2.1.2.7 Scrapping of Dryer Surface 10

2.1.2.8 Cooling of Dryer Chamber Walls 11

2.1.2.9 Admission of Atmospheric Air 11

2.1.2.10 Addition of Drying Aids- Maltodextrin during 11


Spray Drying

CHAPTER III MATERIALS AND METHODS 13-32

3.1 General 13

3.2 Experimental Site Selection 13

3.3 Materials 13

3.3.1 Chemicals 13

3.3.2 Equipment Used 13

3.4 Collection of Sample 22

3.4.1 Juice Preparation 22

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3.4.1.1 Pictorial View for Preparation of Beetroot Juice 23

3.4.2 Powder Preparation 24

3.6 Analysis of Beetroot Juice Powder 27


3.5 Spray Dryer 25

3.6.1.1 Bulk Density 27


3.6.1 Physicochemical Parameters of Beetroot 27

3.6.1.3 Moisture Content on % wet basis 28


3.6.1.2 Moisture Content on % dry basis 28

3.6.1.5 Betalain Content 28


3.6.1.4 Determination of Moisture Ratio 28

3.6.1.7 Yield 29
3.6.1.6 Color 29

3.6.2 Proximate Analysis of Beetroot Powder 30


3.6.1.8 Total Phenolic Compounds 30

3.6.2.2 pH 30
3.6.2.1 Total Soluble Solids 30

3.7 Experimental Design 31


3.6.2.3 Ash Content 30

3.8 Statistical Analysis and Optimization 31

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3.9 Thermal Efficiency of Spray Dryer 32

CHAPTER IV RESULT AND DISCUSSION 33-40

4.1 Laboratory Experimentation 33

4.2 Determination of Physical Parameters 33

4.3 Physical Properties of Vegetables 34

4.3.1 Physical Properties of Beetroot 34

4.4 Chemical Parameters of Beetroot 35

4.5 Physicochemical Properties of Spray Dried 36


Beetroot Juice Powder

4.5.1 Color Determination of Beetroot Juice Powder 36

4.6 Experimental Design 37

4.6.1 Central Composite Design 38

4.7 Thermal Efficiency of Spray Dryer 39

CHAPTER V SUMMARY AND CONCLUSIONS 41-42

REFERENCES 43-48

i
LIST OF TABLES
Table No. Title Page
No.

1.1 Nutritional Value of Beetroot 3

3.1 Specifications of Hunter Color L.a.b 15

3.2 Specifications of Digital pH Meter 15

3.3 Specifications of electronic weighing balance 16

3.4 Specifications of electronic Hot Air Oven 18

3.5 Specifications of Spray Dryer 19

3.6 Specifications of Vernier Calliper 20

3.7 Specifications of Muffle Furnace 21

3.8 Specifications of Refractometer 22

4.1 Physical Parameters of Beetroot 33

4.2 Physical Properties of Beetroot 34

4.3 Chemical Parameters of Beetroot 35

4.4 Physicochemical Properties of Spray dried Beetroot Juice 36


Powder

4.5 Color Determination of Beetroot Juice Powder 37

4.8 ANOVA table showing the variable as linear, quadratic and 38


4.7 Central Composite Design for Beetroot Powder 37
interaction terms on each response variable

x
4.9 Effect of Temperature on the Drying Efficiency 39

4.10 Effect of the Spray Dryer heat on the Drying Effeciency 40

x
LIST OF FIGURES

Fig No. Title Page No.

2.1 Schematic Representation of Spray Drying Mechanism 7

3.1 Food Processing Lab 13

3.2 Mixer Grinder 14

3.3 Hunter Color L.a.b 14

3.4 Digital pH Meter 15

3.5 Digital Weight Balance 16

3.6 Desiccator 17

3.7 Hot Air Oven 17

3.8 Spray Dryer 19

3.9 Digital Vernier Caliper 20

3.10 Muffle Furnace 21

3.11 Refractometer 22

3.12 Fresh Beetroot 23

3.13 Washed and Peeled Beetroot 23

3.14 Sliced Beetroot 23

3.15 Grinded Beetroot 24

3.16 Filtration of Beetroot 24

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3.17 Beetroot Juice Extracted 24

3.18 Spray Dryer 25

3.19 Pictorial view of Spray Dryer, Maltodextrin Concentration, Beetroot Juice 26


Powder

3.20 Bulk density of beetroot Juice Powder, Moisture Content of Powder after26
drying, Ash content

3.21 Desiccator 27

4.1 Variation of pH with respect to Time 35

4.2 Variation of Moisture Content (%db) with respect to Time 36

xi
LIST OF ABBREVIATIONS

Acronym Interpretation

ANOVA Analysis of Variance

AOAC Association of Official Analytical Chemist

BT Betalain

cm Centimeter

db Dry basis

et al. Et alia (and others)

Etc. End of thinking capacity

FAO Food and Agricultural Organization

FFR Feed Flow Rate

GAE Gallic Acid Equivalent

gm Gram

GMD Geometric Mean Diameter

IAT Inlet Air Temperature

i.e. Id est

MC Moisture Content

MD Maltodextrin

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ml Millilitre

mm Millimeter

Pa Pascal

Re Reynolds Number

RPM Revolution Per Minute

RSM Response Surface Methodology

sec Second

t Time

Td Temperature Drop

TPC Total Phenolic Compounds

TSSOT Triguna Sen School of Technology

TSS Total Soluble Solids

wb Wet basis

We Weber Number

x
LIST OF NOTATIONS

Sl. No. Symbol SI Unit Description

o
1 C Temperature

2 % - Percentage

3 + - Plus

4 - - Minus

5 × - Multiplication

6 ± - Plus minus

7 = - Equal

8 < - Less than

9 > - Greater than

10 β - Beta

11 η - Eta

12 ϕ - Phi

13 √ - Square root

14 Ɛ - Epsilon

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ABSTRACT
The present study was aimed to optimize the spray drying process for beetroot juice. Influence of
feed flow rate (8, 10 and 11 mL/min), processing temperature (140, 150 and 160 C) and
maltodextrin concentration (20, 25, and 30%) on packed bulk density, moisture content and

betalain content of beetroot powder were assessed. Also to analyze physical and chemical
composition of beetroot (Beta vulgaris L.). The freshly harvested beetroot selected for evaluation
of different physicochemical and proximate analysis. Results obtained indicated that colour of
beetroot was dark red in colour, length was 16.25 cm, diameter was 5.43 cm, width was 8.33
mm, thickness was 3.83 mm, sphericity index was 66%, surface area was 151.40 mm²,
volume was
143.87 mm³ and mass of beetroot was observed to be 110g. Further, chemical composition of
beetroot was reported and results showed that moisture content was found to be 11.33(%db),
Viscosity was 0.72 Pas. The other proximate parameters such as TSS was found to be 9° Brix,
Ash Content was 1.40% and pH was 6.3.

Now the physicochemical properties of beetroot powder for Bulk density it was found to be 0.65
gm/cm³, Powder yield was experimentally found to be 44.36%, Ash Content was 7.89%. The
following optimum process parameters were determined; feed flow rate feed flow rate of 10
mL/min, processing temperature of 149 C and maltodextrin concentration of 20%. The predicted
values for packed bulk density, moisture content and betalain content were 0.62 g/mL, 6.12 and
33.84 mg/100 g of dry matter, respectively. Within the optimum parameters, the experimental
values for packed bulk density, moisture content and betalain content were 0.62 ± 0.1 g/ mL,
6.10
± 0.1 and 33.14 ± 0.1 mg/100 gm of dry matter.

Keywords: Betalain, Beta vulgaris, Physical Properties, Chemical Properties, Response surface
methodology, Spray-drying, Maltodextrin, Optimization

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CHAPTER – 1

INTRODUCTION
1.1 Background

In tropical, subtropical, temperate and arid regions wide variety and vegetables are
produced in world. Nowadays, the interest of the food industry has significantly increased in
natural flavor and color enriched additives due to the demand of consumers for reducing the use
of synthetic food additives. The beetroot is the taproot portion of a beet plant, usually known in
Canada and the USA as beets while the vegetable is referred to as beetroot in British English,
and also known as the table beets, garden beet, red beet, dinner beet or golden beet. It is one of
several cultivated varieties of Beta vulgaris grown for their edible taproots and leaves (called
beetgreens); they have been classified as B. vulgaris subsp. Vulgaris. Beta is the ancient Latin
name for beets, possibly of Celtic origin, becoming bete in Old English.Root derives from the
late Old English rōt, itself from Old Norse rót.Beets were domesticated in the ancient Middle
East, primarily for their greens, and were grown by the Ancient Egyptians, Greeks and Romans.
By the Roman era, it is thought that they were cultivated for their roots as well. From the Middle
Ages, beetroot was used as a treatment for a variety of conditions, especially illnesses relating to
digestion and the blood. Bartolomeo Platina recommended taking beetroot with garlic to nullify
the effects of "garlic- breath".During the middle of the 19th century, wine often was coloured
with beetroot juice.

Usually the deep purple roots of beets are eaten boiled, roasted, or raw, and either alone or
combined with any salad vegetable. A large proportion of the commercial production is
processed into boiled and sterilized beets or into pickles. In Eastern Europe, beet soup, such as
borscht, is common. In Indian cuisine, chopped, cooked, spiced beet is a common side dish.
Beetroot can be roasted, boiled or steamed, peeled, and then eaten warm with or without butter as
a delicacy; cooked, pickled, and then eaten cold as a condiment; or peeled, shredded raw, and
then eaten as a salad. Pickled beets are a traditional food in many countries. In Poland and
Ukraine, beet is combined with horseradish to form ćwikła or бурачки (burachky), which is
traditionally used with cold cuts and sandwiches, but often also added to a meal consisting of
meat and potatoes. Similarly in Serbia where cvekla is used as winter salad, seasoned with salt

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and vinegar, with meat dishes. As an addition to horseradish, it is also used to produce the "red
variety of chrain, a condiment in

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Process Optimization of Spray Drying of Beetroot

Ashkenazi Jewish, Hungarian, Polish, Lithuanian,Russian, and Ukrainian cuisine. Commonly


used in Australian hamburgers, a slice of pickled beetroot is combined with grilled pineapple,
cooked onion, fried egg on a beef patty to make an "Aussie burger". A common dish in Sweden
and elsewhere in the Nordic countries is Biff à la Lindström, a variant of meatballs or burgers,
with chopped or grated beetroot added to the minced meat.In Northern Germany, beetroot is
mashed with Labskaus or added as its side order. When beet juice is used, it is most stable in
foods with a low water content, such as frozen novelties and fruit fillings.Betanins, obtained
from the roots, are used industrially as red food colourants, e.g. to intensify the colour of tomato
paste, sauces, desserts, jams and jellies, ice cream, sweets, and breakfast cereals.Beetroot can
also be used to make wine.

Raw beetroot is 88% water, 9.6% carbohydrates, 1.61% protein, and less than 1% fat (see
table). In a 100-gram (3+ 1 ⁄2 -ounce) amount providing 180 kilojoules (43 kilocalories) of food
energy, raw beetroot is a rich source (27% of the Daily Value - DV) of folate and a moderate
source (16% DV) of manganese, with other nutrients having insignificant content (table). In
preliminary research, beetroot juice reduced blood pressure in hypertensive people. Tentative
evidence has found that dietary nitrate supplementation, such as from beets and other vegetables,
results in a small improvement in endurance exercise performance. Betanin, obtained from the
roots, is used industrially as red food colorant, to improve the color and flavor of tomato paste,
sauces, desserts, jams and jellies, ice cream, candy, and breakfast cereals, among other
applications. The chemical adipic acid rarely occurs in nature, but happens to occur naturally in
beetroot. For safety: The red colour compound betanin is not broken down in the body, and in
higher concentrations may temporarily cause urine or stools to assume a reddish colour, in the
case of urine a condition called beeturia. Although harmless, this effect may cause initial concern
due to the visual similarity to what appears to be blood in the stool, hematochezia (blood passing
through the anus, usually in or with stool) or hematuria (blood in the urine).Nitrosamine
formation in beet juice can reliably be prevented by addingascorbic acid.

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Process Optimization of Spray Drying of Beetroot

Table 1.1 Nutritional Value of beetroot

Nutrients Value Per 100g

Water 88 %

Protien 1.61 g

Iron 0.80 g

Carbohydrate 9.6 g

Energy 43 kcal

Calcium 16mg

Total Lipid (fat) 0.2 g

Sugar 6.8g

Fiber 2.8 g

Vitamin C 4.9 mg

Calorie 43

Source: [https://www.healthline.com/nutrition/foods/beetroot]

Spray drying is a method of drying of many thermally sensitive materials such as food
and pharmaceuticals in which dry powder from a liquid or slurry by rapidly drying with a hot
gas. Spray drying is a process widely used to produce fruit juice powders and it is the preferred
method (vidya et.al. 2016). Spray drying operations are three steps: (1) atomization of liquid, (2)
drying of droplets, (3) motion of the droplet. The physicochemical properties of Beetroot powder
produced by spray drying depend on some process variables, such as the characteristics of drying
air(Temperature, pressure), liquid feed(Viscosity, particles size, flow rate) and the type of
atomizer. Therefore in order to optimize the drying process to obtain the products with better

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Process Optimization of Spray Drying of Beetroot

sensory and nutritional characteristics with yield (Tonon et al., 2008) . The most of the spray
dried particles is spherical in shape and fluid-like flow properties are provided, which helps in
packaging, pressing, filtering and handling easier and less costly, lower moisture content, lower
hygroscopicity, lower degree of caking and increasing rehydration abilities ( Tonon et al., 2008;
Goula and Adampoulos,2010). The effect of addition of drying aids (Maltodextrin), which have
high molecular weight, avoiding spray drying operational problems during food processing and
storage, such as stickiness on the dryer chamber wall, as well as, structural transformations such
collapse and crystallization on the drying kinetics of low molecular weight sugars and organic
acids( Adhikari et al., 2004).

The optimization of beetroot juice powder was devised using Box-Behnken design to optimize
the spray drying parameters of inlet air temperature (IAT) (160– 180 °C), maltodextrin (MD)
addition rate (5–15%) and feed flow rate (FFR) (400– 600 ml/h). The model to describe and
predict the response in terms of the powder yield, hygroscopicity, redness value, betalain
retention (BR %).

1.2 Objectives

Keeping the above mentioned issues in view, the present study has addressed the following
objectives:

 Determination of physicochemical properties of beetroot, beetroot juice and beetroot


powder.
 To optimize the spray drying process for beetroot juice and study the combined effects of
spray drying parameters.
 To study the proximate analysis of beetroot juice and beetroot powder.

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CHAPTER- 2

REVIEW OF

LITERATURE
2.1 General

This chapter deals with the review of research work carried out by various pioneers on
agricultural spray drying produced fruit juice powder might have some problems with their
property due to the presence of low molecular weight sugars and acids, such as stickiness,
hygroscopic and solubility, which have a low glass transition temperature. The major optimized
parameters in spray drying are inlet air temperature, relative humidity of air, outlet air
temperature, and atomizer speed that are given for a particular study. The juice in spray drying
require addition of drying agents that include maltodextrin, liquid glucose, etc.

2.1.1 Spray dryer

This review describes the different stages of the mechanism of the spray-drying process:
atomization, droplet-to-particle conversion and particle collection. In particular, this work
addresses the diversity of available atomizers, the drying kinetics and the importance of the
configuration of the drying chamber, and the efficiency of the collection devices. The final
properties of the dried products are influenced by a variety of factors, namely the spray dryer
design, the feed characteristics and the processing parameters. The impact of those variables in
optimizing both the spray-drying process and the synthesis of dried particles with desirable
characteristics is discussed.

Kim et al. (2009) and Kha et al. (2010), He reviewed that spray-drying has been
generally utilized for commercial production of fruit powder and also in the production of milk
powder.Spray-dried powders have good reconstitutional characteristics, low water activity and
are suitable for transport and storage.

Sagar and Suresh Kumar (2010), they stated that the advantages of spray drying
include hygienic conditions during processing, low operational costs, and short contact time.
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Process Optimization of Spray Drying of Beetroot

Hennigs et al. (2001), reviewed that during spray drying, sticky products can be
generated, thereby adhering to the internal wall of drying chamber leads to the lower yield).

Ratanasiriwat et al. (2013), stated that the use of high molecular maltodextrin as an
encapsulation or carrier agent in spray drying has been introduced to tackle the problem. It can
also increase the glass transition temperature and stability during storage stated by Fazaeli et al.
(2012).

Tonon et al. (2009), he founded the food powder properties, for example, moisture
content, bulk density and morphology were influenced by gulf temperature. Regularly, the bay
temperature utilizes for spray dry system for sustenance powder is 140–220 C. However
according to scientific literature suitable temperature for spray drying of fruit or vegetable juices
is found in the range 140–180 C.

Samuel Percy (1872) patented that spray drying is a well-known method of particle
production which consists on the transformation of a fluid material into dried particles, taking
advantage of a gaseous hot drying medium. Its first observation is dated 1860 and a primitive
spray dryer device.Ever since it was first discovered, the spray-drying technique has been
improved concerning its operational design and applications. In fact, the primordial spray dryer
devices lacked process efficiency and safety. After overcoming these issues, spray drying
became an attractive method for food industry purposes, ending up to be used in milk powder
production in the 1920s, remaining one of the most important applications until the current days.
Spray-drying evolution was directly influenced by World War II, where there was an imperative
need to reduce the weight and volume of food and other materials to be carried. As a result, spray
drying has become an industry benchmark, namely in the dairy products’ fabrication. In the post-
war period, the spray-drying method continued progressing, reaching the pharmaceutical,
chemical, ceramic and polymer industries. Even after more than a century of research, spray
drying is still a target of study and innovation due to the increasing demand for complex particles
with specific characteristics. This is considered a powerful technological process since it brings
feasibility to the production of free-flowing particles with well-defined particle size. Besides,
bearing in mind the ability to use different feedstocks as well as its high productivity and broad
applications, makes this technique more and more attractive to the scientific community. Spray-
drying mechanism is based on moisture elimination using for that a heated atmosphere to
which the feed product is
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Process Optimization of Spray Drying of Beetroot

subjected. The process may be described by three major phases (atomization, droplet-to-particle
conversion and particle collection), although some authors use four or five minor steps to
describe it in more detail. As shown in Figure 1, a solution is pumped to an atomizer, breaking
up the liquid feed into a spray of fine droplets. Then, the droplets are ejected into a drying gas
chamber where the moisture vaporization occurs, resulting in the formation of dry particles.
Finally, using an appropriate device, the dried particles are separated from the drying medium,
being then collected in a tank.

Figure 2.1: Schematic representation of spray-drying mechanism. (1) Atomization.


(2) Droplet-to-particle conversion. (3) Particle collection.

2.1.2 Basic considerations

2.1.2.1 Spray Drying Steps

Patel et al., (2009), founded that spray drying process mainly involves following five steps:

1. Feedstock is normally concentrated before processing.


2. In second step atomization takes place that creates the optimum conditions for
evaporation to a dried product having a desired characteristics.
3. In third stage atomized liquid is brought into contact with hot gas.
4. Moisture evaporation takes place here in two stages.

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Process Optimization of Spray Drying of Beetroot

5. Keey and Pham (1976) stated that in first stage evaporation takes place at the
constant rate at the surface of droplet. In second stage thetre is no longer enough
moisture to maintain the saturated conditions at the droplet surface. So evaporation
depends on diffusion of moisture through the shell, which is increasing in thickness.
6. Muzafir et al (2016), studied that the separation step takes place for which cyclones,
bag filters, wet scrubbers, and electrostatic precipitators may be used.

2.1.2.2 Operating Conditions

Tonon et al. (2008), reported that the physicochemical properties of powders produced
by spray drying depend on some process variables, such as the characteristics of the liquid feed
(viscosity, particles size, flow rate) and of the drying air (temperature, pressure), as well as the
type of atomizer. Therefore, it is important to optimize the drying process, in order to obtain
products with better sensory and nutritional characteristics and better process yield.

2.1.2.3 Powder Properties

Shrestha et al. (2007), founded that the shape of most spray- dried particles is spherical,
which provides for fluid- like flow properties. This makes many downstream operations, such as
packaging, pressing, filtering, and handling easier and less costly.

Goula and Adamopoulos (2010), they reported that spray drying produces the most
homogeneous product from multi component solutions and slurries. Each particle will be if the
same chemical composition as the mixed feed. Lower moisture content, lower hygroscopicity,
lower degree of caking, and increasing rehydration abilities are the main properties of spray-
dried powder.

2.1.2.4 Stickiness during spray drying

Roos and Karel. (1991), stated that during drying they can stick on the dryer chamber
wall, leading to low product yield and operational problems. The low glass transition
temperature, high hydroscopic, low melting point, and high water solubility of the dry solids
produce the highly sticky products. Stickiness problems can be solved by the addition of some
carrier agents, like polymers and gums, to the product before being atomized.

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Process Optimization of Spray Drying of Beetroot

Jittanit et al. (2010), reported that carrier agent is also used for microencapsulation. It
can protect sensitive food components against unfavorable ambient conditions, mask or preserve
flavours and aromas, reduce the volatility and reactivity and provide additional attractiveness for
the merchandising of food products.

Righetto and Neito, (2005), founded the common carrier agents used for fruit juices are
maltodextrins and gum Arabic. Maltodextrins are products of starch hydrolysis, consisting of D-
glucose units linked mainly by: glycosidic bonds.

Bemiller and Whistler (1996), they described the dextrose equivalence (DE), which is
inversely related to their average molecular weight. Maltodextrins are low cost and very useful
for spray drying process on food materials. Gum Arabic is natural plant exudates of Acacia trees,
which consists of a complex heteropolysaccharide with highly ramified structure.

Rodriguez-Hernandez et al. (2005), stated that it is the only gum used in food products
that shows high solubility and low viscosity in aqueous solution, making easier the spray drying
process. The use of different carrier agents and different drying conditions produces the different
physicochemical properties of powders. Knowledge of food properties is essential to know and
thus will help to optimize the processes, functionalities, to reduce costs, mainly in the case of
powders produced or used in pharmaceutical and food industries.

Verma and S. V. Singh, (2013), stated that properties such as moisture content and
water activity are essential for powder stability and storage. Bulk density is important for
packaging and shipping considerations.

2.1.2.5 Methods of spray drying sugar-rich foods

Bhandari et al. (1997), stated that for sugar-rich food products such as fruit juices, that
are characterized by stickiness and are usually spray dried, common approaches involve
modifying the sticky characteristics of the material most frequently through the addition of
drying aid agents, trying to control the surrounding product or air temperatures, such as using
appropriate outlet drying air temperature or introducing of cold air in to the bottom part of the
dryer or cooling of the wall temperature. The improvement of the spray drying performance
while applying these methods to reduce stickiness has been reviewed elsewhere.

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Process Optimization of Spray Drying of Beetroot

2.1.2.6 Addition of Drying Aids

Tonon et al. (2010), stated that drying aids, which have high molecular weight, aiming at
avoiding spray drying operational problems such as stickiness on the dryer chamber wall, as well
as structural transformations such as collapse and crystallization, during food processing and
storage, which is especially important in the case of sugar rich products such as fruit juices.

Adhikari et al. (2003), stated that the drying aids could form an outer layer on the drops
and alter the surface stickiness of particles due to the transformation into a glassy state.

Grabowski et al. (2006), he studied the changes in surface stickiness reduce the particle
particle cohesion resulting in less agglomeration, and therefore, lower water-holding capacity of
the powders.

Shrestha et al. (2007), reported that the additives must reduce the hygroscopic and
thermoplastic properties of the fruit juice while not alter the quality and solubility of the
produced powder. The use of MDs as drying aids has been in practice since the 1970s used
additives in the research included: MD, liquid glucose, and methylcellulose. Such agents reduce
powder hygroscopicity and increase the glass transition temperature and normally used for
microencapsulation, which can protect sensitive food components against unfavourable ambient
conditions, mask or preserve flavours and aromas, reduce the volatility and reactivity and
provide additional attractiveness for the merchandising of food products.

Silva et al. (2006), studied on the lowest hygroscopicity values were obtained when the
highest MD concentrations were used. As MD concentration increases, the moisture content of
samples significantly reduces. Higher drying aid concentrations favour flowability.

2.1.2.7 Scrapping of Dryer Surfaces

Karatas (1989) developed an experimental spray dryer with a chamber wall scraper for
tomato juice. This method is useful for relatively less thermoplastic sugars such as lactose and
sucrose. Karatas and Esin (1994) investigated the fundamental aspects involved in the drying of
tomato concentrate droplets fully exposed to air of constant humidity and velocity.

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Process Optimization of Spray Drying of Beetroot

2.1.2.8 Cooling of Dryer Chamber Walls

Goula and Adamopoulos, (2010), studied on the cooling of the drying chamber walls is
concerned, the cool wall will be favourable to minimize the thermoplastic particles from sticking,
as the wall will be cold enough to cool and solidify the outer surface of the thermoplastic
particles coming in contact. This method, however, was found to improve the process but not to
resolve the problem. There as on is that the cold chamber wall will also cool the surrounding
environment and cause an increase in the relative humidity of the air close to the wall surface.
Lower temperatures of wall and lower humidities of the drying air resulted in the formation of a
solid particle surface, which decreased residue accumulation or dryer fouling, and minimized the
number of thermoplastic particles sticking to the dryer wall. Masters (1994) modeled a pilot
plant spray dryer with a cooling air jacket that reduced the particle stickiness on the wall.
Masters (1985) introduced chambers with air brooms, which rotates lowly close to the wall, can
also cool the wall surface to prevent stickiness of powders. Mani et al. (2002), reported that the
air broom arm contains a row of nozzles that direct compressed air on to the wall surface.

Sudhagar, (2000), reported that an intermediate sweeping of chamber wall with


dehumidified cold air can remove loosely adhered particles on the chamber wall used air broom
system for spray drying of banana and mango juice. The design aspects of the rotating air broom
system can be found in literature.

2.1.2.9 Admission of Atmospheric Air

Anjali Verma and Satya Vir Singh, (2013), stated that the introduction of cool air at the
lower part of the dryer chamber resulting in the formation of a solid particle surface can also
reduce the stickiness of the powder particles. However, a limited amount of air can only be
introduced because the cooling process will also raise the relative humidity of the air that can
once again aggravate the situation by increasing the surface moisture level.

2.1.2.10 Addition of drying aids-maltodextrin during spray drying

Adhikari et al. (2004), studied that the effect of addition of a drying aid (MD) on the
drying kinetics of low molecular weight sugars and organic acids and on the surface stickiness of
these materials. He conducted single drop drying experiments and developed predictive tools for
prediction of stickiness of drops of binary solutions. He presented the drying kinetics of sugar-

1
Process Optimization of Spray Drying of Beetroot
rich

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Process Optimization of Spray Drying of Beetroot

solutions and acid rich foods including their predicted stickiness history. They conducted
experiments on sugars/ MD mixtures and sugars + citric acid)/ MD mixtures at different
concentrations of MD and analyzed the morphological changes, moisture content changes, and
temperature changes of drop. Addition of MD lowers the drying rate. As the amount of MD in
the drop increases, the surface area increases and diffusion path decreases that enhance the flux
of water leaving the drop. Pure sucrose and fructose drops remain spherical at drying. When the
amount of MD in sucrose or fructose drops is increased to50 %, the drops deviate from sphericity
and become pear-shaped (elongated) after 5 mino f drying. This shape retains throughout the
course of their drying. This shape allows more water to leave the drop and acts to offset the
resistance to moisture diffusion caused by the formation of a skin on the surface. The glass
transition temperature of the surface layer gave quite a reasonable prediction of the surface
stickiness of the mixture drops. The drop surface becomes completely non sticky when surface
layer temperature (TO) exceeds the drop temperature (Td) by 10 C. The presence of acid
prolongs the surface stickiness of sugar-rich foods.

1
CHAPTER- 3

MATERIALS AND METHODS


3.1 General

The chapter includes the experimental site, selection of beetroot, preparation of beetroot
juice powder, determination of physico-chemical properties of beetroot , optimize the process
parameters for the preparation of a beetroot juice powder and determine thermal efficiency of
Spray Dryer. Details of each methodology are explained in the following sections.

3.2 Experimental Site Selection

Fig 3.1- Food Processing Lab

The experimental site is selected in the experimental laboratory of the Department of


Agricultural Engineering Assam University, Silchar.

3.3 Materials

3.3.1 Chemicals

Maltodextrin reagent is used for avoiding stickiness.

3.3.2 Equipment Used

Mixer Grinder, hunter color l.a.b, pH meter, digital weight balance, desiccators, hot air
oven, conical flask, tissue paper, hand gloves, funnel, measuring cylinders, beaker, crucible,
thong, magnetic stirrer, knife, peeler, plates, strainer, Petri plates, spray dryer, Digital vernier
calliper, muffle furnace, refractometer.

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Process Optimization of Spray Drying of Beetroot

3.3.2.1 Mixer Grinder

Fig 3.1 – Mixer Grinder

A mixer grinder helps to reduce manual work and saves time. From pureeing, mixing,
grinding, mincing to chopping, the mixer grinder is designed for multiple tasks and gives a fine
product without clear pieces.

3.3.2.2 Hunter Color L.a.b

Fig 3.2- Hunter Color L.a.b

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Process Optimization of Spray Drying of Beetroot

Table 3.1-Specifications of Hunter Color L.a.b

Sl. No. Parameter Details

1 Measurement Principle Tristimulus Colorimeter

2 Photometric range 0-125%

3 Lamp Life Approx 1000hrs

4 Measurement time Less than 1 sec

The Hunter is a filter colorimeter which separates the components of reflected color into a 3
dimensional color scale. The L,a,b color scale views color in a similar manner to which the
human eye sees color, with L measuring light to dark color components, a is a red-green scale
and b is a yellow-blue scale.

3.3.2.3 Digital pH Meter

Fig 3.3- Digital pH Meter

Table 3.2- Specifications of Digital pH Meter

Sl. No. Parameter Details

1 Range 0-14pH

2 Probe pH electrode

3 Relative Humidity 5-90% non- condensing

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Process Optimization of Spray Drying of Beetroot

4 Power 230V and 50 Hz

PH meter, electric device used to measure hydrogen-ion activity (acidity or alkalinity) in


solution. Fundamentally, a pH meter consists of a voltmeter attached to a pH-responsive
electrode and a reference (unvarying) electrode.

3.3.2.4 Digital Weight Balance

Fig 3.4- Digital Weight Balance

Table 3.3: Specifications of electronic weighing balance

SL. No. Parameters Details

1 Brand Aczet

2 Model No CG 302

3 Capacity Max- 300g and Min- 0.5 g

4 Platter size 118 mm

5 Display 7 digit

6 Display type LCD

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Process Optimization of Spray Drying of Beetroot

7 Power source 6V

An electronic balance is a device used to find accurate measurements of weight. It is used very
commonly in laboratories for weighing chemicals to ensure a precise measurement of those
chemicals for use in various experiments.

3.3.2.5 Desiccators

Fig 3.5- Desiccator

A desiccator is an air-tight enclosure that can be used in two methods. The first method is
to remove moisture inside the desiccator to prevent moisture from damaging moisture sensitive
samples such as electronics and chemical samples that may react to moisture.

3.3.2.6 Hot Air Oven

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Process Optimization of Spray Drying of Beetroot

Fig- 3.6 Hot Air Oven

Table 3.4: Specifications of hot air oven

Sl. No. parameters Details

1 Manufacturer LABARD INSTRUCHEM


PVT. LTD.

2 Drying chamber type Stainless steel

3 Temperature range 50 to 250℃

4 Temperature accuracy ± 2℃

5 No. of trays 2 nos.

6 Power supply 230 V AC, 50 Hz

Hot air ovens use extremely high temperatures over several hours to destroy microorganisms and
bacterial spores. The ovens use conduction to sterilize items by heating the outside surfaces of
the item, which then absorbs the heat and moves it towards the centre of the item.

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Process Optimization of Spray Drying of Beetroot

3.3.2.7 Spray Dryer

Fig 3.7- Spray Dryer

Table 3.5- Specifications of Spray Dryer

Sl. No. Parameters Details

1 Voltage 240V

2 Power 2900 W

3 Electric Current 12A

4 Diameter of Chamber 0.1 m

5 Maximum Temperature Drying 220° C

Spray drying is a method of producing a dry powder from a liquid or slurry by rapidly drying
with a hot gas. This is the preferred method of drying of many thermally-sensitive materials such
as foods and pharmaceuticals or materials which may require extremely consistent, fine, particle
size. There are three fundamental steps involved in spray drying. 1) Atomization of a liquid
feed into

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Process Optimization of Spray Drying of Beetroot

fine droplets. 2) Mixing of these spray droplets with a heated gas stream, allowing the liquid to
evaporate and leave dried solids. 3) Dried powder is separated from the gas stream and collected.

3.3.2.8 Digital Vernier Calliper

Fig 3.8- Digital Vernier Calliper

Table 3.6: Specifications of digital vernier calliper

SL. No. Parameters Details

1 Brand KRISTEEL

2 Model No 2916/ 2917

3 Measuring range 0-150 mm and 0-200 mm

4 Resolution 0.01 mm/ 0.0005”

5 Display LCD

6 Power SR 44. One 1.55 V Button


cell

A Digital Vernier calliper is a device used to measure the dimensions of an object. The tip of the
calliper is adjusted to fit across the points to be measured and the dimension read by measuring
between the tips with another measuring tool, such as a ruler.

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Process Optimization of Spray Drying of Beetroot

3.3.2.9 Muffle Furnace

Fig 3.9- Muffle Furnace

Table 3.7- Specifications of Muffle Furnace

Sl. No. Parameters Details

1 Maximum Temperature 900-1700° C

2 Power 3-4 Kw

3 Heating Rate 20-25 J/m

4 Insulation Time 0-999 min

Muffle furnaces now use technology and design to achieve greater control of temperature
uniformity and isolate heated materials from combustion contaminants. This makes muffle
furnaces ideal for ashing samples, heat-treating applications, and materials research.

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Process Optimization of Spray Drying of Beetroot

3.3.2.10 Refractometer

Fig 3.10- Refractometer

Table 3.8- Specifications of Refractometer

Sl. No. Parameter Details

1 Display Touch Screen

2 Refractive Index 1.3000 to 1.7000

3 Weight 2Kg

4 Dimension 329mm×214mm×150mm

A refractometer is used to measure the amount of sugar in a solution. This is done based on the
refraction index of the liquid. More sugar in solution will produce a higher refraction index. The
scale of the refractometer is calibrated to read the equivalent concentration of sugar for a given
refraction index.

3.4 Collection of Sample

100% fresh beetroot (Beta vulgaris L.) was purchased from local market.

3.4.1 Juice Preparation

Raw material for the study was 100% fresh beetroot juice. Fresh and uniform sizes of
round shaped beetroot were procured from the local market, (Irongmara, Silcher). Care was
taken to ensure that there was no bruising, cutting or any sign of physical injury. Beetroot were

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Process Optimization of Spray Drying of Beetroot
washed in

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Process Optimization of Spray Drying of Beetroot

running water and cleaned properly and then juice was extracted by juicer. Extracted beetroot
juice was filtered with the help of muslin cloth. Maltodextrin used as a drying agent was
procured from a local supplier.

Flowchart

Sorting

Washing

Peeling

Rewashing

Weighing

Slicing (2-3 mm)

Juice extracted

Filtration using muslin cloth

3.4.1.1 Pictorial View for Preparation of Beetroot Juice

Fig 3.11 Fresh Beetroot Fig 3.12 Washed and Peeled Fig 3.13 Sliced Beetroot

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Process Optimization of Spray Drying of Beetroot

Fig 3.14 Grinded Beetroot (a) Fig 3.15 Grinded Beetroot (b) Fig 3.16 Filtration

Fig 3.17 Beetroot Juice Extracted

3.4.2 Powder Preparation

The drying of prepared juice blended with drying agents was carried out in a laboratory
scale spray dryer. The powder obtained from spray drying was collected in the cyclone, then
transferred to glass twist-off jars.

Flow chart

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Process Optimization of Spray Drying of Beetroot

Juice ectraction

Mix Maltodextrin reagent

Stir thoroughly

Spray drying

Beetroot powder is obtained

Packaging

Sealing

Storing at room temperature

3.5 Spray dryer

Fig 3.18 – Spray Dryer

Powder will produce using a Laboratory Spray dryer (LSD-1). The spray dryer operates
concurrently downwards and has a spray nozzle, two-fluid atomizer. The inlet air temperature

2
Process Optimization of Spray Drying of Beetroot
was

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Process Optimization of Spray Drying of Beetroot

140-180ºC for all the solutions and outlet air temperature 107ºC. Beetroot juice was fed into the
drying chamber using a peristaltic pump. Water evaporation capacity 1lit/hr. Power supply of
Spray dryer is 230 V, 50Hz. Spray nozzles: 2 Fluid nozzles. Air flow: downward concurrent.
Feed pump: Peristatic pump with controller for regulating the feed rate to the nozzle. The
product obtained will vacuum sealed in polyethylene bags. The bags will then store in a
desiccators containing silica gel before quality evaluation.

Fig 3.19- Pictorial view of Spray Dryer, Maltodextrin Concentration, Beetroot Juice Powder

Fig 3.20- Bulk density of beetroot Juice Powder, Moisture Content of Powder after drying, Ash
content

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Process Optimization of Spray Drying of Beetroot

Fig 3.21- Desiccator

3.6 Analysis of beetroot juice powder

The prepared beetroot juice powder was analysed for different physicochemical
properties such as packed bulk density, moisture content, betalain content, color, yield, total
phenolic compounds, ash content, total soluble solid.

3.6.1 Physicochemical Parameters of beetroot and beetroot Powder

The physical parameters of the sample was analysed using standard methods. Physical
properties such as length, width, thickness, size, geometric mean diameter, surface area,
sphericity, weight was determined to analyse the dimension.

3.6.1.2 Weight

The weight of the individual samples and total samples were determined using an electronic
balance to an accuracy of 0.001g.

3.6.1.2 Bulk density

The packed bulk density was determined by measuring tare weight of 100-mL cylinder.
The powders were consolidated by tapping on a rubber mat until the volume was reduced and
reasonably constant. The bulk density was calculated by dividing the mass of the powder by the
volume that occupied the cylinder (Goula et al. 2008). The volume of the powder was read in mL
and bulk density recorded as g/ml.

3.6.1.3 Moisture content on % dry basis

Moisture content of the powder sample will be determined according to AOAC method
(2012). Fifteen runs of different weight of each powder sample 1.5- 2.0 gm will take and dried in
3
Process Optimization of Spray Drying of Beetroot

a vacuum oven at a temperature of 70ºC until a constant weight obtained. The samples will
analyse and the mean was recorded.

Initial weight of sample (gm)−Dry weight of the sample(gm)


Mc (db) (%) = Initial weight of the sample × 100

3.6.1.4 Moisture content on % wet basis

Moisture content on % wet basis can be calculated using the Eq.

weight of wet sample (gm)−Dry weight of the sample(gm)


Mc (wb) (%) = weight of dry sample × 100

3.6.1.5 Determination of the moisture ratio

The moisture ratio of beetroot during the drying can be calculate using

𝑀−𝑀𝑒
M.R =𝑀𝑜−𝑀𝑒

Where, M = Moisture content at any drying time (% dry basis),

Mo = Initial moisture content (% dry basis),

Me = Equilibrium moisture content (% dry basis)

The value of Me is relatively small compared with M and Mo especially for food materials
(Junling et al., 2008). Therefore, Me can be assumed to be zero, hence the MR can be simplified
to equation below.

M.R = 𝑀
𝑀𝑜

3.6.1.5 Betalain content

Quantification of betalain (BT) was performed by the spectrophotometric method as


described by Cai and Corke (1999) and Cassano et al. (2007) using UV–Vis spec- trophotometer.
Pigments were extracted from the sample with methanol at pH 6.5. The determination of betalain
concentration, i.e. violet and yellow pigments, was calculated in terms of betacyanin (BC) and
indicaxanthin-I (IX) respectively. The betalain content collectively along with betacyanin and
indicaxanthin, expressed as mg/L, and was calculated individually by using the following
equation proposed by Cai and Corke (1999).

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Process Optimization of Spray Drying of Beetroot

𝐴 ×𝐷𝐹 ×𝑀𝑊 ×1000


B= Ɛ ×𝐿

Where A is the absorption for betacyanins and indicaxanthins; DF is the dilution factor
and L is the path length of the cuvette (1cm). For MW and Ɛ, the molecular weights and
extinction coefficients of the representative compounds betacyanin and indicaxanthin have been
considered (Cai and Croke 1999; Cassano et al. 2007).

3.6.1.6 Colour

The color of the fresh juice and reconstituted samples will be analyzed using a hunter
color lab and the difference in their color parameters was calculated with the Hunter values (L, a,
b) the optical parameters were compared. Fifteen measurements were recorded for each sample
and their mean values calculated. The color values represented whiteness or brightness/darkness
(L), redness/greenness (a) and yellowness/blueness (b). Another informative attribute in the
production of beetroot juice is the total color difference (ΔE) which is a combination of
parameters L, a and b (Maskan, 2006). Total color change parameters commonly used to
characterize the variation of color in powder and are calculated as:

ΔE= √(𝐿˳ − 𝐿𝑡 )² + (𝑎˳ − 𝑎𝑡)² + (𝑏˳ − 𝑏𝑡)²

Where,

L˳= L before drying, Lt= L after drying

a˳= a before drying, at= a after drying

b˳= b before drying, bt= b after drying

3.6.1.7 Yield

The weight of the dry material in the power produced and the juice consumed was used to
determine the spray drying yield. This factor was calculated from the following equation:
P ×Sp
Yield= × 100
𝐿×𝑆𝑓

Where P is the rate of powder production (gm/min), Sp is the percent of total solids of the
powder (%), L is the feed flow rate (gm/min), and Sf is the percent of total solids of the feed (%)
(Chegini and Ghobadian. 2007).

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Process Optimization of Spray Drying of Beetroot

3.6.1.8 Total phenolic compounds

The total phenolic content was determined by spectrophotometry, following the Folin-
Ciocalteu method, with the same modifications of Ruiz-Gutierrez et al. (2014). Measurements
were performed in triplicate using a gallic acid curve as a standard. It was used a
spectrophotometer 765 nm. Results were expressed in mg of gallic acid equivalents (GAE)/100g
powder.

3.6.2 Proximate analysis of beetroot powder

The beetroot powder was analysed for total soluble solids, PH, Ash content.

3.6.2.1 Total soluble solids

TSS measure the sugar content of sugar solutions in which the sugar is the major
component using refractometer. Total soluble solids content of beetroot solution is determined by
the index of refractometer, and is referred to as the degrees a Brix. A drop of solution was place
on the refractometer prism and light beam was passed through the prism and the results obtained
were noted down. After every reading it was cleaned with distilled water and dried with tissue
paper.

3.6.2.2 pH

A digital PH meter composed of two electrodes i.e., calomel electrode and glass
electrodes were used to determine the pH of beetroot solution. First the electrode was clean with
tissue paper and standardized with buffer solution of pH 4. Then the sample was placed on glass
for few seconds. The glass electrode was cleaned with distilled water and dried with tissue paper
after every reading.

3.6.2.3 Ash content

In this method, a muffle furnace is used to burn down the dry powder taken in a crucible.
The temperature of the chamber is maintained approx. 550° c. At this temperature, the water
evaporates from the sample and rest of the contents burn down. The percentage of ash content
was calculated as:

Ash content (%) = (Weight of ash (gm)) / (Weight of sample (gm)) × 100

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Process Optimization of Spray Drying of Beetroot

3.7 Experimental Design

Response surface methodology (RSM) is an important tool in analysing the experimental


data, resulting in the optimization conditions for product development. It is used for
simultaneous optimization of multiple process variables to achieve desired response variables,
RSM was used to derive the optimum process conditions using a three-parameter five level
central composite rotatable design giving 16 experimental runs including 5 replicates at the
centre point. The independent variables affecting the quality of the end product were the inlet air
temperature and maltodextrin concentration. Response variables including moisture content, total
color change, and rehydration ratio were used as quality characteristics of beetroot juice powder.

The response variables included packed bulk density, moisture content and betalain
content. The second-order polynomial equation was fitted to the experimental data of each
dependent variable.

Yku = βk0 + 𝑛
𝛽𝑘𝑖𝑋𝑖𝑢 + 𝛽𝑘𝑖𝑖𝑋2𝑖𝑢 + ∑𝑖=0 𝛽𝑘𝑗𝑋𝑖𝑢𝑋𝑗𝑢 + 𝐸𝑘𝑢
∑𝑛 𝑖
∑𝑛 𝑖
∑𝑛 𝑖

where term Yku is response variable, Y1u is packed bulk density (g/mL of beetroot
powder). Y2u is moisture content (%wb), Y3u is betalain content of the beetroot powder. Where,
βk0 is the value of the fitted response at the centre point of the design, i.e. point (0,0) and βki,
βkii and βkj are the linear, quadratic and interactive regression terms, respectively.

3.8 Statistical analysis and Optimization

All experiments will conduct in triplicate and an analysis of variance will performed. The
least significant difference at p< 0.05 will calculated using the Duncan Multiple Range Test on
Minitab software. The data were expressed as mean ±SD.

The main aim of the optimization of the spray drying process for beetroot juice was
focused to discover the levels of independent variables such as feed flow rate, processing
temperature and maltodextrin %, which would result in minimum packed bulk density, minimum
moisture content and maximum betalain content of beetroot powder. To achieve this goal, a
criterion was adopted by selecting lower and upper limit for individual parameter to achieve the
maximum desirability. By using this approach, observed values were compared with predicted

3
Process Optimization of Spray Drying of Beetroot
values for each parameter. According to these parameters desirability of model was found and
corresponding to the maximum

3
Process Optimization of Spray Drying of Beetroot

desirability of the values of different parameters such as feed flow rate, processing temperature
and maltodextrin % were noted.

3.9 Thermal efficiency of Spray Dryer

Heat utilization efficiency (η) of spray dryer is expressed as,

Amount of heat utilized by liquid drops


η = Amount of heat energy supplied to ambient air

MₐCpₐ(Ti−To)
η = MₐCpₐ(Ti−Tambient)

Where

Ti= Inlet temperature,

To= Outlet temperature,

Tambient= Ambient temper

3
CHAPTER- 4

RESULT AND

DISCUSSION
This chapter describes result and discussion about the findings of physical properties,
combined effects of the spray-drying parameters including feed flow rate, processing
temperature and maltodextrin to maximize the moisture content of the beetroot (beta vulgaris)
juice powder and determination of thermal efficiency of Spray Dryer of powder production.

4.1 Laboratory Experimentation

In order to carry out the laboratory experiment for spray drying of beetroot juice powder,
proximate analysis, physicochemical properties such as color, moisture content, ash content,
betalain content, total soluble solid, pH were determined using standard methods and techniques.

4.2 Determination of Physical

Parameters Table 4.1- Physical

Parameters of Beetroot

Physical Parameters Units Average Value

Mass Gm 110

Length Cm 16.25

Diameter cm 5.43

Shape - Round

Colour - Dark Red

Viscosity Pa s 0.72
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Process Optimization of Spray Drying of Beetroot

4.2 Physical properties of Vegetables

The physical property such as length, width, thickness, geometric mean diameter, surface
area, sample weight, seeds, density, thickness, sphericity were determined using standard
methods. The results obtained for beetroot are presented in the table 4.2.

Table 4.2- Physical Properties of Beetroot

Sample Major Intermediate Minor GMD Sphericity Surface Volume


no Axis axis axis index(Ø) area (S)
(Dg) (V)
Length(L) Width(W)(m thickness (mm²)

(mm) m) (T)(mm) [(L*W*T (mm3)
)⅓]
(mm)

1 9.87 7.41 3.25 6.18 62.6 120.09 93.84

2 10.15 7.90 3.58 6.58 64.9 136.30 121.23

3 10.46 8.25 3.92 6.95 66.4 151.84 144.25

4 10.80 8.85 4.05 7.26 67.3 165.90 165.72

5 11.09 9.25 4.37 7.62 68.8 182.87 194.30

Average 10.47 8.33 3.83 6.92 66.0 151.40 143.87

Mean 10.47 8.33 3.83 6.92 66.0 151.40 143.87

SD 0.49 0.73 0.43 0.56 2.37 24.54 38.85

4.2.1 Physical properties of Beetroot

The average, minimum and maximum length of beetroot observed are 10.47, 9.87, 11.09
mm respectively while the average, minimum and maximum width of beetroot observed are
8.33, 7.41, 9.25mm respectively. The average, minimum and maximum thickness of beetroot
observed is 3.83, 3.25, 4.37mm respectively.

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Process Optimization of Spray Drying of Beetroot

The average, minimum & maximum geometric diameter of beetroot observed are 6.92, 6.18,
and 7.62 mm respectively. The average, minimum, and maximum surface area of beetroot
obtained are 143.87, 93.84, 194.30 mm^2 respectively. The average, minimum, and maximum
sphericity obtained is 66, 62.6, 68.8 respectively. (Table 4.2)

4.3 Chemical Parameters of Beetroot

The chemical parameters such as betalain content, total soluble solid, pH, ash content,
moisture content were determined using standard methods. The results obtained for beetroot are
presented in the table 4.3.

Table 4.3- Chemical Parameters of Beetroot

Sample Betalain TSS (°Brix) pH Ash Content Moisture


Content (%) Content
(%db)

1 9 6.5 1.42 13.34

2 9 6.3 1.49 12.02

3 9 6.4 1.38 11.22

4 9 6.3 1.40 11.08

5 9 6.3 1.41 9.12

Mean 9 6.3 1.40 11.33

6.55
6.5
6.45
6.4
6.35
6.3
6.25
p

6.2

1 2 3 4 5

Time (hr)

Fig 4.1- Variation of pH in Beetroot Juice with respect to Time

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Process Optimization of Spray Drying of Beetroot

14

12

10
Moisture Content

0
1 2 3 4 5

Time (hr)
Fig 4.2- Variation of Moisture Content with respect to Time

4.4 Physicochemical properties of spray dried beetroot juice powder

Table 4.4- Physicochemical properties of spray dried beetroot juice powder

Bulk Density Powder Yield (%) Ash Content

Powder Volume Predicted Experimental Mass Mass


(gm) (cm³) dry ash
(gm) (gm)

2.6 4 46.094 44.35 100 7.89

0.65 7.89%

4.4.1 Colour Determination of Beetroot Juice Powder

Measurements for beetroot juice powders are shown in Table (4.5). L-value measures the
lightness of the sample, +a measures the red colour and + b measures the yellow colour. This
result shows when inlet air temperature increased, the b values and a values decreased. The
maximum color difference was observed at the highest temperature. This may be due to the
sensitivity of color pigments to the heating process and the diluting effect of maltodextrin
(colourless) in color found for spray drying of beetroot juice powder.

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Process Optimization of Spray Drying of Beetroot

Table 4.5 – Colour Determination of Beetroot Juice Powder

S.L No. Inlet air L a b ᴧE


temperature
(°C)

1 50 20.103 12.467 5.567 24.300

2 65 19.037 11.163 3.260 22.307

3 80 16.423 10.127 2.643 19.473

4 100 17.043 9.880 2.903 19.913

4.5 Experime4ntal Design

4.5.1 Central Composite design with experimental values of response variables for Beetroot
Powder

Response surface methodology was used to investigate the optimum combination of


spray drying conditions on the physicochemical properties of the spray-dried powders. A central
composite design with three variables, feed flow rate, processing temperature and maltodextrin
concentration shown in Table 4.7.

Table 4.8 shows the ANOVA data for response variable and its significance along with
correlation coefficients. A high correlation coefficient explained the goodness of fit of the
experimental data in the response surface models.

Table 4.7- Central composite design for Beetroot Powder

Run no. Feed flow Processing Maltodextrin Packed Moisture Betalain


rate temperature (%), (X3) bulk content, content
(mL/min), (°C), (X2) density (%) (mg/100gm
(X1) (g/mL) of dry matter)

3
Process Optimization of Spray Drying of Beetroot

Due to 2nd wave of covid-19, further experiment was not carried out as University
restricted entry for the visitors.

The tabular form in which the data was to be kept is given below:

Table 4.8 ANOVA table showing the variable as linear, quadratic and interaction terms on each
response variable

Source df Bulk density (g/mL) Moisture content Betalain


(%) content
(mg/100gm of
β F P β F P dry matter)
Value value Value Value

Model

A-feed flow
rate

B-processing
temperature

C-malto
dextrin %

3
Process Optimization of Spray Drying of Beetroot

AB

AC

BC

Residual

Lack of fit

Pure error

Cor total

4.6 Thermal Efficiency of Spray Dryer

The main factors affecting the thermal efficiency are the inlet air temperature, outlet air
temperature and environment temperature. There are several measures for the reduction of heat
consumption in spray drying process is heat utilized in the drying process and heat supplied by
the drying process.

Table 4.9- Effect of Temperature on the drying efficiency

S.L no. Inlet air Outlet air Ambient Thermal


temperature (°C) temperature (°) temperature (°C) Efficiency (%)

1 154.0 68.5 26 66.7

2 120.0 61.7 31 65.5

3 170.4 78.7 30 65.3

4 148.0 67.8 27 66.2

5 182.4 82.7 31 65.8

3
Process Optimization of Spray Drying of Beetroot

Average 65.9

Table 4.10- Effect of the Spray Dryer heat on the Drying Efficiency

S.L no. Heat Supplied Heat Consumed Thermal Efficiency


(%)
Voltage Ampere Watt

1 57.5 26.5 3000 50.79

2 53.7 27.8 3000 49.76

3 60.0 25 3000 50.0

4 68.5 30 3000 68.5

5 72 28.4 3000 68.91

4
CHAPTER- 5

SUMMARY AND

CONCLUSION
5.1 Summary

The well-documented health benefits of a diet high in fruit and vegetables has led to a
growing interest in so-called “functional foods” and their application in health and disease. In
recent years, the root vegetable Beta vulgaris rubra, otherwise known as red beetroot (herein
referred to as beetroot) has attracted much attention as a health promoting functional food. While
scientific interest in beetroot has only gained momentum in the past few decades, reports of its
use as a natural medicine date back to Roman times. Today, beetroot is grown in many countries
worldwide, is regularly consumed as part of the normal diet, and commonly used in
manufacturing as a food colouring agent.

The physical properties of beetroot revealed the average, minimum and maximum length
of (10.47, 9.87, 11.09) mm, width of (8.33, 7.41, 9.25)mm, thickness of beetroot observed is
(3.83, 3.25, 4.37)mm respectively.

The average, minimum & maximum geometric diameter of beetroot observed are 6.92,
6.18, and 7.62 mm, surface area of beetroot obtained are 143.87, 93.84, 194.30 mm^2, sphericity
obtained is 66, 62.6, 68.8 respectively.

Chemical composition was reported and results showed that moisture content was found
to be 11.33(%db), Viscosity was 0.72 Pas. The other proximate parameters such as TSS was
found to be 9° Brix, Ash Content was 1.40% and pH was 6.3.

The physicochemical properties of beetroot powder for Bulk density it was found to be
0.65 gm/cm³, Powder yield was experimentally found to be 44.36%, Ash Content was 7.89%.
The following optimum process parameters were determined; feed flow rate feed flow rate of 10
mL/min, processing temperature of 149 C and maltodextrin concentration of 20%. The predicted
values for packed bulk density, moisture content and betalain content were 0.62 g/mL, 6.12 and
33.84 mg/100 g of dry matter, respectively. Within the optimum parameters, the experimental
values for packed bulk density, moisture content and betalain content were 0.62 ± 0.1 g/ mL,
6.10
± 0.1 and 33.14 ± 0.1 mg/100 gm of dry matter.
41
Process Optimization of Spray Drying of Beetroot Juice

Note- Further process optimization of spray drying of beetroot juice could not be fulfilled
due to the 2nd wave of covid-19, since entry of the students was restricted inside the
University Campus.

5.2 Conclusion

It could be finally concluded that beetroot is good source of protein, carbohydrate and
dietary fibre. Beetroot is good source of minerals such as sodium and potassium. The beetroot is
good source of betalain, which makes it potential source for exploration and value addition in
food beverages in combination with various fruit juices.

Although thesis is a scientific work done by the students which is basically done to reveal
the phenomenon, facts and issues to be analyzed to give a conclusion from the result of the
analysis.

As research can be done by field study and library studies, so some of the parameters
could not be analysed because of this global pandemic, since the entry of the students in our
University Campus was restricted.

42
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