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# Institution of Chemical Engineers
Trans IChemE, Vol 81, Part C, June 2003

www.ingentaselect.com=titles=09603085.htm

THE USE OF EXPERIMENTAL FACTORIAL DESIGN FOR

ANALYSING THE EFFECT OF SPRAY DRYER OPERATING
VARIABLES ON THE PRODUCTION OF TOMATO POWDER
S. AL-ASHEH, R. JUMAH, F. BANAT and S. HAMMAD
Department of Chemical Engineering, Jordan University of Science and Technology, Irbid, Jordan

two-level factorial experimental design technique was used to investigate the in uence
of the operating parameters on the production of tomato powder from tomato paste
during the spray drying operation. This technique was applied to quantify the in uence
of feed total solids, feed ow rate, inlet air temperature and air ow rate on the process
variables, namely, product total solids, particle size, bulk density and solubility. A factorial
model was constructed and used to study all interactions among the considered parameters. The
results showed that, at a 95% con dence interval, the effect of air ow rate was relatively
insigni cant, while the effects of feed total solids, feed ow rate and inlet air temperature were
at the same signi cance level. Most interactions between the studied parameters were
insigni cant.
Keywords: spray drying; tomato powder; factorial design.

Convective dehydration is another technique for tomato

drying. Tomatoes are washed, cut and then typically
passed through long tunnels where they are dehydrated by
warm air. This process is quite capital-intensive but the
process is easier to control. Dehydrated tomatoes produced
by this method have less than 7% moisture, a less sharp
taste, and lighten slightly in color after 1215 months
storage.
Among the industrial dryer types available, there are a
few that accept pumpable food material suspensions at the
dryer inlet and discharge a dry particulate at the outlet.
Spray drying is a unique technique which is able to produce
powder of speci c particle size and moisture content irrespective of dryer capacity and product heat sensitivity. In
many cases, spray drying is the only rational choice to dry
uid feedstocks (Masters, 1985).
Spray drying refers to the removal of moisture from a
slurry by breaking it into small droplets in the presence of
hot air to obtain a solid, dry powder. In the spray-drying
process, the liquid feed is pumped into the drying chamber
through an atomizing system. Inside the drying chamber, a
stream of heated gas traps the droplets and carries them
from the drying chamber to the product recovery system.
Evaporation takes place in a few seconds as the relatively
cool droplets come in contact with the hot gas.
Tomatoes have very low solid content, less than 6%. Spray
drying must be preceded by evaporating the pulped tomato
to produce a paste containing 30% solids (Greensmith,
1998). The physical form of tomatoes, as a powder, provides
a stable, natural, easily dosable ingredient which may be
used to impart color and taste for food products (Bhandari
et al., 1993).

INTRODUCTION
The world annual production of tomatoes is about 100.7
million metric ton and is considered one of the important
food products. Jordan produces annually about 0.3 million
metric ton (FAO, 2001), in four different areas and seasons.
The southern part of the Jordan valley produces tomatoes in
January and February, the middle part of the Jordan valley in
May and June, the northern part of the Jordan valley in June
and July, and the hilly areas in July and November. It is
estimated that about 37% of Jordans tomatoes are produced
as triple-concentrated tomato paste (Amitom, 2001).
Preservation of tomatoes is of commercial importance. It is
used as a component in various vegetable and spicy dishes
and, in many countries, canned tomato is one of the main
canned vegetable products. It is characterized by its taste,
color and avor, and providesseveral vitamins, e.g. vitamin C,
carotenes and other valuable nutrients (Baloch et al., 1997).
Powdered tomato has many advantages, including ease of
packing, transportation and mixing, and no drum-clinging
loss (Masters, 1985). In addition, tomato powder is much in
demand by dehydrated soup manufacturers. It is now
produced in many countries where tomatoes are an indigenous outdoor crop (Greensmith, 1998).
Tomatoes can be sun-dried, dehydrated or spray-dried. The
oldest technology is sun drying, where ripened tomatoes are
rst washed, halved and then usually kept in a water bath
containing sulfur dioxide. They are then transferred into
drying trays which are exposed to the sun for 710 days.
Thereafter, they are cut and packaged. The result is a
product with typically 1224% moisture, robust in taste,
which darkens after an expiry time of 912 months.
81

AL-ASHEH et al.

82

The objective of this work is to study the effect of

operational variables such as feed concentration, feed ow
rate, air ow rate and inlet air temperature on product
tomato powder properties including total solids, particle
size, bulk density and solubility. The study was performed
using the two-level factorial experimental design. The
interaction among the variables is also considered.
MATERIALS AND METHODS
Preparation of Tomato Paste Feed
Tomato paste purchased from the market and consisting
of 25% solids was used as a feed to the spray dryer. It was
diluted to the required feed concentration by addition of
distilled water.
Spray Drying Process
The tomato paste was spray-dried using a pilot spray
dryer (Mobile Minor, Niro Atomizer, Seborg, Denmark)
with a vaned centrifugal atomizer driven by an air turbine.
The drying chamber is 800 mm in diameter, 600 mm
cylindrical height and conical based. The cone angle is
60 . All internal surfaces that contact the product are
stainless steel AISI 316. The nominal atomizer wheel
supplied with the unit rotates within the range 25,000
35,000 rpm.
The feed, at speci c concentration, was introduced and
metered into the dryer by means of a peristaltic pump
(Watson Marlow 503 S) in the range 816 ml min1 and
atomized into ne droplets using the wheel atomizer. The
drying air was electrically heated and controlled at the
speci ed temperature. It entered the drying chamber through
a ceiling disperser designed to create a swirling air ow
directly around the vaned atomizer wheel. A schematic
diagram of the experimental set-up is shown in Figure 1.

Product Analysis
Product total solids
A sample of tomato powder (about 12.0 g) was weighed
and placed in an oven at 105 C for 24 h. The total solid
percentage (weight basis) was calculated as:
Total solids (%)

weight of dried sample

100 (%)
weight of sample

Particle size
Average particle diameter of the product was measured
using a particle size analyser (Fritsch analyser).
Bulk density
The bulk density of the product was determined by
pouring about 5 g of the powder into a 10 ml graduated
cylinder. The volume occupied by the sample was recorded
and bulk density was calculated (Wade and Waller, 1994).
Solubility
The solubility of the product was measured using the
method adopted by Wade and Waller (1994). Saturated
solutions were prepared by adding 7, 8, and 9 g of tomato
powder into 100 ml distilled water. These solutions were left
for 48 h to ensure equilibrium. Then they were ltered, and
their absorbance was read at 328 nm wavelength. A calibration curve was prepared from which the solubility of the
samples was calculated.
TWO-LEVEL FACTORIAL EXPERIMENTAL DESIGN
The response variables in this study are the product total
solids (y1), particle size ( y2), bulk density ( y3), and solubility ( y4). In order to determine the effect of the operating

Figure 1. Schematic diagram of the spray drying process.

Trans IChemE, Vol 81, Part C, June 2003

EXPERIMENTAL FACTORIAL DESIGN

Table 1. Values of operating variables in the designed set
of experiments.
Operating variable
x1 (feed total solids), %
x2 (feed ow rate), ml min1
x3 (inlet air temperature), C
x4 (air ow rate), cm3 s1

4.66
8
130
630

9.11
16
160
800

83

where the parameter bi is responsible for the in uence of the

operating variables xi on the response yi, while bij, bijk and
bijkl are responsible for the possible interactions, among
operating variables, on the response. Values of these 16
parameters can be obtained by least square estimates.
Using the matrix X of the operating variables at different
runs and Y as the matrix of the response variable for this
process, the least square tted model, according to equation
(1), provides:
y1 98:1325 0:3712x1 0:6325x2 0:3038x3
0:0112x4 0:1288x1 x2 0:0275x1 x3

variables on the response variables, a set of designed

experiments was performed. Two feed total solids (x1),
two feed ow rates (x2), two inlet air temperatures (x3),
and two air ow rates (x4) were selected to perform a twolevel factorial design for the present study. Each of these
operating variables was selected at lower and upper levels
and expressed in the following dimensionless form:

0:005x1 x4 0:0438x2 x3 0:0188x2 x4

0:01x3 x4 0:0325x1 x2 x3 0:025x1 x2 x4

0:0062x1 x3 x4 0:015x2 x3 x4
0:0012x1 x2 x3 x4

{value of operating variable i}

(1=2){its upper limit its lower limit}
xi
(1=2){its upper limit its lower limit}

y2 4:9681 0:5494x1 2:2881x2 0:7119x3

0:0131x4 0:0531x1 x2 0:0656x1 x3

0:0419x1 x4 0:2794x2 x3 0:0156x2 x4

Therefore, each variable is ranked as 1 and 1 at lower

and upper levels, respectively. For ease of notation, the
effects were designated as in Table 1, which shows the
values of the operating variables selected in this study.

0:0106x3 x4 0:0106x1 x2 x3 0:0419x1 x2 x4

0:0206x1 x3 x4 0:0044x2 x3 x4
0:0169x1 x2 x3 x4

(3)

y3 0:5962 0:0575x1 0:05x2 0:0238x3

0:0012x4 0:0038x1 x2 0:0025x1 x3

RESULTS AND DISCUSSION

0:0075x1 x4 0:005x2 x3 0:0012x3 x4

A 2 complete factorial design can be performed with the

values of the operating variables shown in Table 1. This
results in 16 tests with all possible combinations of x1, x2, x3
and x4. The response variables, y1, y2, y3 and y4 were
measured for each of these tests as shown in Table 2.
Replicates for some runs for the purpose of statistical
analyses are shown in Table 3.
The complete factorial model that can be used to t the
data in Table 2 is:

0:0038x1 x2 x3 0:0038x1 x2 x4 0:0025x2 x3 x4

0:0038x1 x2 x3 x4

(4)

y4 0:03968 0:00166x1 0:00176x2 0:00291x3

0:00021x4 0:00022x1 x2 0:00025x1 x3
0:00018x2 x3 0:00002x2 x4 0:00006x1 x2 x3
0:00009x1 x2 x4 0:00004x1 x3 x4

0:00006x2 x3 x4 0:00005x1 x2 x3 x4

E(Yi ) b 0 b1 x1 b2 x2 b3 x3 b4 x4 b12 x1 x2
b13 x1 x3 b14x1 x4 b23 x2 x3 b24x2 x4

(5)

Estimation of Interaction Effects

b34 x3 x4 b123 x1 x2 x3 b124 x1 x2 x4

b234x2 x3 x4 b134 x1 x3 x4 b1234x1 x2 x3 x4

(1)

The interaction effect is calculated as the average

response difference between one half of the factorial runs

Table 2. Experimental results of 24 designs for the response variables.

Test no.

x1

x2

x3

x4

y1 (%)

y2 (mm)

y3 (g cm3)

y4 (g ml1)

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1

97.57
97.52
97.02
96.92
98.5
98.56
97.93
98.07
98.13
98.17
97.31
97.36
99.54
99.5
98.97
99.05

7.74
7.61
5.89
5.80
2.51
2.40
1.65
1.75
8.71
8.93
6.57
6.80
3.75
3.79
2.82
2.77

0.55
0.57
0.60
0.62
0.46
0.47
0.52
0.52
0.70
0.69
0.74
0.70
0.58
0.56
0.63
0.63

0.0425
0.0430
0.0360
0.0359
0.0460
0.0465
0.0400
0.0408
0.039
0.0395
0.0334
0.0340
0.0420
0.0422
0.0368
0.0372

Trans IChemE, Vol 81, Part C, June 2003

(2)

AL-ASHEH et al.

84

Table 3. Experimental results of replicates.

Repeated test
2
10
12
14

y1 (%)

y2 (mm)

y3 (g ml1)

y4 (g ml1)

97.52
97.41
97.63
98.17
98.26
98.08
97.36
97.3
97.42
99.5
99.47
99.53

7.61
7.45
7.77
8.93
8.75
9.11
6.80
6.71
6.89
3.79
3.90
3.68

0.57
0.57
0.57
0.69
0.67
0.71
0.75
0.72
0.78
0.56
0.58
0.54

0.0430
0.0422
0.0438
0.0395
0.0410
0.0380
0.0340
0.0332
0.0348
0.0422
0.0420
0.0424

and the other half. The design table must be augmented to

include columns for interactions. An interaction column is
formed from the column of the two factors, three factors
or four factors that comprise the interaction, by multiplying the entries in the factor column. This is shown in
Tables 47.
It is seen that all three-variable and four-variable interactions are insigni cant. Only the interaction between x1 and
x2 has an effect on y1, and the interaction between x2 and x3
has an effect on y2. Other two-variable interactions are
insigni cant. Evidence of large negative (x1x2 in y1) and
positive (x2x3 in y2) interaction is strong and therefore
cannot be neglected from the model.
Estimation of Main Effects
From a statistical point of view, the main effect can be
estimated from the difference between the average high-and
low-factor-level responses,
P
{response
at high xi }
P
{response at low xi }
main effect of xi
(1=2){the number of factorial runs}
(6)
Thus, all experimental data (Tables 2 and 3) are used to
estimate each main effect which is estimated independently
of the other main effects. This feature of 2n design is
known as a hidden replication, giving maximum information per experimental run (Murphy, 1976). A summary
of the calculation procedure is shown in Tables 47 for
the response variables y1, y2, y3 and y4, respectively,
where the average response has been taken for the replicate runs.
Therefore, the effect of increasing the feed total solids
from 4.66 to 9.11%, averaged over all levels of feed ow
rate, inlet air temperature and air ow rate is to increase
product total solids by 0.7425%, increase particle size by
1.099 mm, increase bulk density by 0.115 g cm3, and to
decrease solubility by 0.00332 g ml1. Also, the effect of
increasing the feed ow rate from 8 to 16 ml min1 is to
decrease product total solids by 1.265%, increase particle
size by 4.576 mm, increase bulk density by 0.1 g cm3, and
decrease solubility by 0.00352 g ml1. The effect of increasing inlet air temperature from 130 to 160 C is to increase
product total solids by 0.6075%, increase particle size by

Standard deviation

Degrees of
freedom (mi1)

y1

y2

0.11

0.16

0.0008

0.09

0.18

0.02

0.0015

0.06

0.09

0.03

0.0008

0.03

0.11

0.02

0.0002

y3

y4

1.424 mm, decrease bulk density by 0.0475 g cm3, and

increase solubility by 0.00582 g ml1. Finally, increasing
air ow rate from 630 to 800 cm3 s1 has only a slight
effect on the response variables: product total solids
decreases by 0.0225%, particle size decreases by
0.0262 mm, bulk density increases by 0.0025 g cm3, and
solubility decreases by 0.00042g ml1.
In another study (Banat et al., 2002) these in uences have
been investigated individually rather than using two level
factorial design. It was found that the increase in the feed
total solids increased tomato powder total solids, particle
size and bulk density, while the increase in the feed ow rate
decreased tomato powder total solids and solubility, and
increased particle size and bulk density. These conclusions
are consistent with the results of factorial design obtained in
this work.
Increasing the feed total solids, i.e. decreasing the moisture content, decreases the drying loads which ease the
production of dried product. The increase in particle size
with the increase in the feed total solids is not entirely due to
the larger volume occupied by the higher solids concentrations. The actual particle size is apparently in uenced by the
physical properties of the feed, mainly viscosity (Wallman
and Blyth, 1951). The increase in the feed concentration
causes an increase in viscosity. The particles formed are
heavy-walled spheroids and become solid spheres, having a
relatively high bulk density (Chu et al., 1951). Furthermore,
larger particles have a larger diffusion boundary layer,
retarding transport of dissolved material from the particle
surface (Brittian, 1995).
The increase in feed ow rate results in a decrease in
product total solids and solubility, and an increase in particle
size and bulk density. Increasing feed ow rate increases the
amount of water introduced to the dryer, which consequently increases the water content of the product and
thus decreases product total solids. The increase in particle
size does not necessarily indicate that larger droplets were
formed as they left the atomizer wheel. This increase in
particle size could be due to the greater probability of
collision and subsequent coalescence of the droplets
(Wallman and Blyth, 1951). Powder bulk density increases
with feed ow rate as a result of higher water content of the
product particles because water has a higher density
compared to the dry solid (Jumah et al., 2000). The decrease
in solubility is due to the increase in particle size as
explained earlier.
Trans IChemE, Vol 81, Part C, June 2003

Trans IChemE, Vol 81, Part C, June 2003

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
788.03
782.09
0.7425

x1

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
780
790.12
1.265

x2

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
787.49
782.63
0.6075

x3
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
784.97
785.15
0.0225

x4
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
784.03
786.09
0.2575

x12
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
785.28
784.84
0.055

x13
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
785.02
785.1
0.01

x14

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
44.14
35.35
1.099

x1

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
58.05
21.44
4.576

x2

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
45.44
34.05
1.424

x3
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
39.64
39.85
0.026

x4
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
39.32
40.17
0.106

x12
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
40.27
39.22
0.131

x13
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
39.41
40.08
0.084

x14

S corresponds to the sum of responses at high xi, while S corresponds to the sum of responses at low xi.

7.74
7.61
5.89
5.80
2.51
2.40
1.65
1.75
8.71
8.93
6.57
6.80
3.75
3.79
2.82
2.77
Sa
Sa
Difference effect

y2 (mm)

Operating factors

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
785.41
784.71
0.0875

x23
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
785.21
784.91
0.0375

x24
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
785.14
784.98
0.02

x34

Dummy factors

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
41.98
37.51
0.559

x23

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
39.62
39.87
0.031

x24

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
39.83
39.66
0.021

x34

Dummy factors

Table 5. Calculations and results for main effects for the response variable y2.

S corresponds to the sum of responses at high xi, while S corresponds to the sum of responses at low xi.

97.57
97.52
97.02
96.92
98.50
98.56
97.93
98.07
98.13
98.17
97.31
97.36
99.54
99.50
98.97
99.05
Sa
Sa
Difference effect

y1 (%)

Operating factors

Table 4. Calculations and results for main effects for the response variable y1.

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
39.83
39.66
0.021

x123

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
785.32
784.8
0.065

x123

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
39.41
40.08
0.084

x124

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
784.86
785.26
0.05

x124

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
39.71
39.78
0.009

x234

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
784.94
786.18
0.03

x234

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
39.58
39.91
0.041

x134

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
785.11
785.01
0.0125

x134

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
39.88
39.61
0.034

x1234

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
785.07
785.05
0.0025

x1234

EXPERIMENTAL FACTORIAL DESIGN

85

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
5.23
4.31
0.115

x1

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
5.17
4.37
0.1

x2

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
4.58
4.96
0.0475

x3
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
4.78
4.76
0.0025

x4
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
4.80
4.74
0.0075

x12
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
4.79
4.75
0.005

x13
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
4.83
4.71
0.015

x14

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3041
0.3307
0.332

x1

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3033
0.3315
0.352

x2

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3407
0.2941
0.582

x3
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3157
0.3191
0.0425

x4
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3192
0.3156
0.045

x12
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3154
0.3194
0.05

x13
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3174
0.3174
0

x14

S corresponds to the sum of responses at high xi, while S corresponds to the sum of responses at low xi.

0.0425
0.0430
0.0360
0.0359
0.0460
0.0465
0.040
0.0408
0.039
0.0395
0.0334
0.034
0.0420
0.0422
0.0368
0.0375
Sa
Sa
Difference effect 102

y4 (g ml1)

Operating factors

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
4.81
4.73
0.01

x23
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
4.77
4.77
0

x24
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
4.76
4.78
0.0025

x34

Dummy factors

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3188
0.316
0.035

x23

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3176
0.3172
0.005

x24

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3174
0.3174
0

x34

x123

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3169
0.3179
0.0125

x123

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
4.8
4.74
0.0075

Dummy factors

Table 7. Calculations and results for main effects for the response variable y4.

S corresponds to the sum of responses at high xi, while S corresponds to the sum of responses at low xi.

0.55
0.57
0.60
0.62
0.46
0.47
0.52
0.52
0.70
0.69
0.74
0.70
0.58
0.56
0.63
0.63
Sa
Sa
Difference effect

y3 (g cm3)

Operating factors

Table 6. Calculations and results for main effects for the response variable y3.

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3167
0.3181
0.0175

x124

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
4.8
4.74
0.0075

x124

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3169
0.3179
0.0125

x234

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
4.75
4.79
0.005

x234

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3177
0.3171
0.0075

x134

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
4.77
4.77
0

x134

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.3178
0.317
0.01

x1234

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
4.74
4.80
0.0075

x1234

86
AL-ASHEH et al.

Trans IChemE, Vol 81, Part C, June 2003

EXPERIMENTAL FACTORIAL DESIGN

Increasing inlet air temperature from 130 to 160 C results in
an increase in product total solids, particle size and solubility, and a decrease in bulk density. It is obvious that at lower
temperatures the rate of heat transfer decreases and thus
drying becomes less complete than at higher temperatures
(Chu et al., 1951). The decrease in bulk density with
increasing air inlet temperature, although partly due to
decreased moisture, is due to case hardening of the droplet
at higher temperatures followed by expansion of the
entrapped vapor (Wallman and Blyth, 1951). Case hardening would explain the increase in particle size with inlet air
temperature. Also, coarse particles t together more loosely,
while small particle pack together with fewer voids. Looser
packing means lower bulk density (Deis, 1997). Case hardening is a phenomenon associated with many fruit and
vegetables powders. Tomato paste is a lm forming material
where drying rate can drop to zero; when evaporation rate
from the surface of the particle is higher than the rate of
moisture supply from the interior to the surface of the drying
material, the surface layer becomes substantially dried. This
causes a shell volume at the surface to form an impermeable
crust that encapsulates the moisture in the interior (Karatas
and Esin, 1994). The increase in solubility with inlet air
temperature was not completely understood. This requires
further investigation.
As for air ow rate, it can be concluded that it has no
signi cant effect on any of the response variables. Evaporation from the surface is enhanced by improved convective
mass transfer rates as a result of increased air velocity. Thus,
increasing air velocity shortens the constant drying rate
period, which is typically quite short in spray drying operations, lasting perhaps for a few seconds. Consequently, most
of the drying occurs in the falling rate period. Here, the rate
of moisture transport from within the droplet surface limits
the amount of moisture lost to the drying air and drying is
not limited by external conditions. Thus, increasing air ow
rate has little effect on nal product total solids. The rate of
air ow controls to a certain extent the residence time of the
products in the drying chamber. The increase in the residence time leads to a greater degree of moisture removal
while reducing air velocity assists product recovery from the
drying chamber (Jumah et al., 2000).
It can also be observed that the in uence of feed ow rate
on product total solids is greater than that of feed total solids
followed by inlet air temperature. As for product particle
size, feed ow rate has the greatest effect followed by inlet
air temperature followed by feed total solids. Feed total
solids has the greatest effect on bulk density followed by
feed ow rate followed by inlet air temperature. Finally, it
can be seen that the in uence of inlet air temperature on
solubility is greater than that of feed ow rate followed by
feed total solids.
The effects of dummy factors can be similarly calculated.
These factors represent a measure of any interactions in the
system. It is seen that some of these interaction factors are
signi cant compared to the effects of the main operating
variables, therefore their in uence on responses cannot be
neglected.
Assessment of Signi cance of Main Effect
To explore the importance of each term in equation (3), a
con dence interval can be calculated for each parameter
Trans IChemE, Vol 81, Part C, June 2003

87

associated with that term. If the con dence interval for a

given parameter contains the point zero, it means that the
term associated with such parameter is not important and
can be excluded from the model [equation (1)]. The con dence interval for the least square parameter estimates is
given by (Montgomery and Runger, 1994):
=
b^ i tn,a [V (b^ i )]1 2

(7)

where tn,a is the Students statistic, n is the degrees of

freedom associated with the pure error variance, s2, and a
is the probability limit. The pooled variance, s2p , can be used
as an estimate of the pure error variance and is given by:
Pl
(mi 1)s2i
2
sp Pi1
(8)
l
i1 (mi 1)

where l is the total number of replicates available in the data

set (i.e. l 4), mi, is the number of data points in the ith set
of replicates and s 2i is the estimate of the pure
P errorl variance
in the ith set of replicates. The term
i 1 (mi 1)
represents the degree
associated with s2p . The
P n of freedom
sample variance [ i 1( yi y)2=(n 1)] can be used as an
estimate of the variance s2i . Therefore, the resulting degrees
of freedom is n 8 and an estimate of pure error variance
for y1 is s2p 0:006175, for y2 it is s 2p 0:01955, for y3 it is
s2p 0:000425, and for y4 it is s2p 8:925 107 . Since
V b^ of each parameter estimate in equation (3) is s2=24,
then the 95% con dence interval for each parameter in each
response variable, according to equation (7) is: for y1
b 0.0453; for y2b 0.0806; for y3b 0.0119; for
y4b 0.00054.
Applying these values of con dence interval, equations
(2)(5) reduce to:
y1 98:1325 0:3712x1 0:6325x2 0:3038x3
0:1288x1 x2

(9)
y2 4:9681 0:54938x1 2:2881x2 0:7119x3
0:2794x2 x3
(10)
y3 0:5962 0:0575x1 0:05x2 0:0238x3
(11)
y4 0:03968 0:00166x1 0:00176x2
0:00291x3

(12)

It can be concluded that for all four variables neither the

effect of x4 (air ow rate) nor its interactions with other
variables are signi cant at 95% con dence interval. It is also
seen that equations (11) and (12), which represent the tted
model for responses variables y3 and y4, respectively, do not
contain any interaction terms. The interaction effect is
obvious in y1 (product total solids) and y2 (particle size);
y1 is affected by the interaction between x1 and x2, while y2
is affected by the interaction between x2 and x3.
CONCLUSIONS
Experiments on the production of tomato powder from
tomato paste were conducted using a spray dryer. The main
effects and interactions among the studied parameters such
as feed total solids, feed ow rate, inlet air temperature, and
air ow rate on tomato powder properties, including total
solids, particle size, bulk density and solubility, were
analysed using a two-level factorial design model. It was

AL-ASHEH et al.

88

found that increasing feed total solids increased tomato

powder total solids, particle size and bulk density and
decreased its solubility. Increasing feed ow rate decreased
tomato powder total solids and solubility and increased the
average particle size and bulk density. Feed temperature
increased particle size and decreased bulk density. Inlet air
temperature had an effect of increasing product total solids,
particle size and solubility, and decreasing bulk density. The
effect of the parameters was assessed at 95% con dence
interval. It was found that air ow rate had no signi cant
effect, at 95% con dence interval, on response variables at
the range of air ow rate used. It was also found that feed
ow rate had the greatest effect on product total solids and
particle size. Feed total solids had the greatest effect on bulk
density and inlet air temperature had the most pronounced
effect on powder solubility. The interaction between feed
total solids and feed ow rate had a slight effect on product
total solids, while only the interaction between feed ow rate
and inlet temperature had a slight effect on product particle
size. No other interactions among the parameters were
observed in the other response variables.
REFERENCES
Amitom, 2001, www.tomate.org=Amitom.htm, Jordan.
Baloch, W.A., Khan, S. and Baloch, K., 1997, In uence of chemical
additives on stability of dried tomato powder, Int J Food Sci Technol,
32: 117120.
Banat, F., Jumah, R., Al-Asheh, S. and Hammad, S., 2002, Effect of
operating parameters on the spray drying of tomato pase, Eng Life Sci,
2: 15.
Bhandari, B., Senoussi, A., Dumoulin, E. and Lebert, A., 1993, Spray drying
of concentrated fruit juices, Drying Technol, 11(5): 10811092.

Brittian, H.G., 1995, Physical Characterization of Pharmaceutical Solids

(Marcel Dekker, New York), pp 179180.
Box, G.E.P. and Hunter, J.S., 1961, The 2ki fractional factorial designs,
part I, Technometrics, 3: 311351.
Chu, J.C., Stout, L.E. and Bushe, R.M., 1951, Spray drying of santomerse,
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Deis, R., 1997, www.foodproductdesign.com
FAO, 2001, www.apps.fao.org=default.htm, Italy.
Greensmith, M., 1998, Practical Dehydration, 2nd edition (CRC Press,
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Jumah, R., Tashtoush, B., Shaker, R. and Zraiy, A., 2000, Manufacturing,
parameters and quality characteristics of spray dried jameed, Drying
Technol, 18(45): 967984.
Karatas, S. and Esin, A., 1994, Determination of moisture diffusivity
behavior of tomato concentrate droplets during drying in air, Drying
Technol, 12(4): 799822.
Masters, K., 1985, Spray Drying Handbook, 4th edition (John Wiley and
Sons, New York), p 5 and 618.
Montgomery, D.C. and Runger, G.C., 1994, Applied Statistics and
Probability for Engineers (John Wiley and Sons, New York).
Murphy Jr., T.D., 1976, Design and analysis of industrial experiments, Chem
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Wade, A. and Waller, P.J., 1994, Handbook of Pharmaceutical Exipient, 2nd
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ADDRESS
Correspondence concerning this paper should be addressed to
Dr S. Al-Asheh, Department of Chemical Engineering, Jordan University
of Science and Technology, P.O. Box 3030, Irbid 22110, Jordan.
E-mail: alasheh@just.edu.jo
The manuscript was communicated via our Regional Editor Professor
J. A. Howell. It was received 16 May 2002 and accepted for publication
after revision 3 April 2003.

Trans IChemE, Vol 81, Part C, June 2003