Professional Documents
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03-326
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INTRODUCTION
Mango (Mangifera indica L.) is commonly referred as the king of the tropical fruits
because of its palatability. In most tropical countries, it is processed at raw and ripe
stages as jam, pickle and beverages. The total world production is about 24 million tones
(FAOSTAT, 2000). In the recent years, mangoes have become well established in the
global market. Today, the consumption of processed mango products such as mangoflavored beverages either singly or multi-flavored beverages is rapidly increasing in the
western hemisphere, thus the demand for processed pulp (puree) had dramatically
increased.
Many food materials have distinct physical characteristics in addition to their
nutritional values; most often it is the rheological characteristic that makes significant
contributions to the overall quality of the product (Rielly 1997). For example, to the
consumer, the flow characteristics of some products (tomato ketchup, sauces, mayonnaise
etc) may be as important as the taste; similarly the mouth feel (determined by its
rheological properties) may contribute as much to the pleasure of eating, as does the
flavor.
concentration, temperature (Rao, 1995), and because of their wide variation of structure
and composition, foods may exhibit flow behavior ranging from simple Newtonian to
time-dependent non-Newtonian and viscoelastic (Singh and Heldman, 1993). A nonNewtonian fluid exhibits shear thinning behavior and their viscosities decreases with
increase in shear rate. Mango puree was reported to be pseudo-plastic (shear thinning)
and thixotropic fluid with yield stress (Gunjal and Waghmare, 1987; Manohar et al.,
1990; Bhattacharya, 1999). The rheological properties obtained from rheometer test may
be represented in terms of constitutive equations between the rate of strain in the fluids
and the applied shear stress. Power law models with or without yield stress has been
extensively used to model the flow behavior of fruit purees.
Whole mango consists of about 82% water, 0.2% fat and about 14%
carbohydrates (Holland et al. 1991). Mango puree like many other fruit purees are
usually stored in the frozen state. Frozen food materials often exhibits phase transition
typical of amorphous polymers (Parks and Thomas 1934; Roos 1987; Slade and Levine
1991). During storage food may loose its integrity as a result of unstable molecular
transformation (Aguilera and Stanley 1999). A different form of quantifying water
mobility and food stability was necessary thus the application of the concept of glass
transition was introduced in food science (White and Cakebread 1966). In storing food
below glass transition temperature (Tg), the rate of any type of changes is severely
reduced and the product becomes virtually stable, while the molecular mobility is
restricted (Jorge et al. 1999).
Differential scanning
In spite
flow rates in pipes, pump sizes, mixing, and heat transfer for concentration, dehydration,
pasteurization, and sterilization (Holdsworth 1971). Another important practical
application ids the determination of suitable quality control parameters for example,
consistency index (Tiu and Boger, 1974).
Sample preparation
Tommy Atkins Mango (Mangifera Indica L.) variety was acquired from local dealer. The
fruit was produced in Mexico. The ripen mango fruits was washed and peeled manually
and the flesh was sliced from the seed carefully and placed in a blender. The puree was
filled into a sterilized glass jars hermetically sealed and was heated in a water bath at
80C for 15 min. The samples were refrigerated at 4C till the next step. To acquire
different levels of mango puree concentrations sugar was added, and thoroughly mixed.
Chemical analysis
The pH was determined by using pH meter (Accumet meter, model 25, Denver
Instrument Company, Arvada, CO). The total soluble solids (TSS) was measured using a
hand refractometer (model ATC, 0.90%), Shilac, Japan).
Rheological measurement
A controlled stress rheometer (AR2000, TA Instruments LTD, Leatherhead, UK) with a
standard steel parallel plate (40 mm) geometry coupled with a built-in peltier plate
temperature control was used. Flow curves were generated by using both the controlled
shear-rate and controlled shear-stress, hence, viscosity was determined from shear
stress/rate curves at different temperatures. Time-dependency (thixotropy) was measured
at different temperatures. Different combinations of shear rates and temperature ram
were used to measure viscosity.
For each test, samples were placed between the parallel plates and allowed two
min to equilibrate prior to all test operations. The data were logged automatically during
the test by a microcomputer attached to a rheometer. The rheograms (flow curves) were
directly fitted to the desired mathematical models by the software (TA instrument
advantage software) based on the Herschel-bulkleys model (eq. 1):
= 0 + k& n
(1)
where is shear stress (Pa), 0 is the yield stress (Pa), k is the consistency coefficient,
and & is the shear rate (s-1).
Thermal analysis
Differential scanning calorimeter (DSC) (Q100-Tzero technology, TA Instruments INC.,
New Castle, DE) equipped with a refrigerated cooling system (RCS) consting of two
stages, cascade and vapor compression refrigeration system with an attached cooling
head, which operates within the ranges of 90 to 550C was used for the this experiment.
The DSC was operated through a microcomputer. Nitrogen (Ultra high purity 5) was
used as the purged gas and the flow rate was 50 mL/min at 138 kPa (20 psi).
Sample
sizes of 12 to 16 mg were weighed into the hermitic pans and sealed. The samples were
encapsulated in aluminum hermitic pans with the aid of the TA instrument Q series
sample encapsulating press with the hermitic sealing die attachment. The cell resistance
and capacitance, cell constants and temperature calibrations were accomplished by
running empty pans, sapphire and indium (melting point 156.6C). The heating rate was
5C/min within the temperature range of 90 to 100C. The thermograms were generated
with the software (TA instrument advantage software).
Experimental design
The central composite rotatable design (CCRD) (Box and Draper 1987) was used
for the rheology study. The CCRD consisted of a three-factored factorial with two levels.
The factors and their levels are shown in Table 1.
Table 1. Coded and uncoded levels of three predictor variables for mango puree.
Varaibles
Levels
Midlevel
Semi-range
70
45
25
12
24
18
300
800
550
250
-1
Temperature (C)
20
Concentration (Brix)
-1
Shear Rate (s )
The matrix for the CCRD optimization experiment is summarized in Table 2. The
CCRD design has eight experimental points in a cube (run No. 1-8), six star points with
an axial distance of 1.682 (run No. 9-14), 3 replications at the central point of the design
5
(run No. 15-17) for experimental error determination. All the experimental units (run)
were replicated 3 times.
A full second-order polynomial model of the type shown in Eq. 2 was used to
evaluate the yield (response variable, y) as a function of dependent variables (x) namely
temperature (C) (denoted by subscript 1), concentration ( Brix) (denoted by subscript
2), shear rate (s-1) (denoted by subscript 3) and their interactions.
y = b0 + b1 x1 + b2 x2 + b3 x3 + b12 x12 + b13 x13 +
b23 x23 + b1 x12 + b22 x22 + b33 x32
(2)
The results were analyzed using the Statistical Analysis System (SAS v.8) software.
Non-linear regression analysis (Marquardt Hougaard) was used for estimating the
consistency index (k).
Table 2. Selected factors and their levels for the first factorial design with the CCRD
design.
Standardized Coded Levels
Run
Concentratio
Temperature
X1
X2
X3
Shear Rate
n
(C)
(S-1)
(Brix)
1
-1
-1
-1
20
12
300
-1
-1
70
12
300
-1
-1
20
24
300
-1
70
24
300
-1
-1
20
12
800
-1
70
12
800
-1
20
24
800
70
24
800
1.682
87
18
550
10
-1.682
18
550
11
1.682
45
28
550
12
-1.682
45
550
13
1.682
45
18
970
14
-1.682
45
18
130
15
45
18
550
16
45
18
550
17
45
18
550
(p>0.05) on effect flow behavior index, revealed by the regression analysis. These results
are in conformity with that of Manohar et al. (1990) on mango pulp concentrate. Based
on the flow behavior index (n), mango puree used in this study was characterized as a
shear thinning fluid.
Table 3 Second order design matrix and rheological parameters: flow behavior index
(n), yield stress ( 0 ) and consistency coefficient (K).
Coded
Parameters
(Pa)
(pa sn)
0.377
7.46
9.01
0.412
3.46
4.31
0.406
8.23
9.37
0.445
3.68
4.56
0.412
3.79
5.04
-1.4
0.391
11.49
13.50
1.4
0.418
5.33
6.55
-1.4
0.436
2.51
3.03
0.393
6.81
7.20
10
0.405
6.21
7.41
11
0.414
6.02
7.69
Run
X1
X2
X1*X2
X1
X2
-1
-1
-1
-1
-1
-1
1.4
The main effects of temperature, concentration and shear rate on viscosity of mango
puree were investigated using response surface analysis.
generated and the parameters that were not significant were dropped from the regression
equation. The analysis of variance shows significant (p < 0.001) quadratic effects of the
main variables effects and no significant (p > 0.05) interaction of cross products. The
lack of fit was also significant (p>0.05). Equations 3 to 5 were used to predict the
rheological parameters of mango puree at various independent variables used in this
study. The second-order surface models derived from the regression analysis are as
follows:
Viscosity
Viscosity was computed based on the Herschel-bulkleys model and response surface
analysis was used to characterize the effect of concentration (Brix) and shear rate as
shown in Fig. 1. The predictive equation for viscosity was acquired from a non-linear
equation as shown in Eq. 3:
(R
= 0.98
(3)
10
Vi scosi t y
0. 400
0. 217
0. 033
- 0. 150
30
1000
16
Concent r at i on
525
Shear Rat e
2 50
Fig. 1 Effect of concentration (Brix) and Shear rate (s-1) on viscosity of mango puree.
Yield stress
The yield stress was obtained for experimented data (shear stress vs. shear rate), which
best fitted the Herschel-bulkleys models.
conducted with the yield stress data and the predictive equation is shown as follows (Eq.
4):
(4)
11
and decreases at high shear rates. Yield stress ranged from 2.5 to 11(Pa) in this study for
mango puree. Our values were lower than those reported by Manohar et al. (1990) that
ranges from 2 to 180 Pa, while greater than those reported by Bhattacharya (1999) (0.8 to
4 Pa).
Yi el d St ess
12
30. 0
-3
90. 0
17. 5
C
oncent r at i on
47. 5
Tem
per at ur e
5. 0 5. 0
Fig. 2 Effect of temperature and concentration (Brix) on yield stress of mango puree.
Consistency index
The consistency values were computed for shear stress and shear rate data by nonlinear
regression analysis. A predictive model was generated through response surface analysis.
(R = 0.96)
(5)
12
15. 00
8. 33
1. 67
- 5. 00
90. 0
30
16
Concent r at i on
47. 5
Tem
per at ur e
5. 0 2
13
followed by a decrease in rate, which confirms that mango puree exhibits shear thinning
behavior with time as also shown in Fig. 1.
90.00
80.00
70.00
60.00
50.00
40.00
30.00
20.00
10.00
0
200.0
400.0
600.0
shear rate (1/s)
800.0
1000
1200
14
T1
T2
(Brix)
10
12
20
28
30
T3
TC
Tm
(mg)
(C)
-63.85
-60.07
-55.50
-56.93
-51.70
-57.09
-50.96
-55.25
-50.35
-51.63
-46.47
Sample Mass
-15.75
3.50
(3.0406) (0.3041)
-14.00
2.64
(0.4243) (0.6505)
-15.68
1.37
(0.3567) (0.4164)
-17.60
0.34
(0.7071) (0.1202)
-17.77
0.28
(1.1504) (0.2013)
15.35
12.3
12.3
13.8
14.05
T1=Onset glass transition temperature, T2 = midpoint glass transition temperature, T3 end point glass
transition temperature, TC = crystallization temperature and Tm = melting temperature; Standard deviation
in parenthesis.
15
The effect of soluble solid concentration on mango puree crystallization appeared rather
erratic, although, it tends to increase with increase in concentration, probably due to
decreased water activity of the product.
0.5
-0.5
-1.5
Mango 30
Mango 12
Mango 20
Mango 28
Mango 10
-2.5
-3.5
-40
-20
20
40
Temperature (C)
Exo Up
product
stored
from
this
region.
16
-0.05
Mango 30
Mango 12
Mango 20
Mango 28
Mango 10
-0.10
-0.15
-0.20
-0.25
-90
Exo Up
-80
-70
-60
Temperature (C)
-50
-40
Universal V3.7A TA Instruments
Fig. 6 Glass transition profiles for mango puree at different TSS concentration.
CONCLUSIONS
The flow behavior index (n) varies from 0.37 to 0.44 and does not significantly change at
all levels of total soluble solid concentration range used in this study. Mango puree was
found to be thixotropic time-dependent fluid. The crystallization and melting peaks were
affected by the change in total soluble solid concentration of the mango puree. The glass
transition temperature increases from 60 to 52C from concentration 10 to 30Brix
respectively.
ACKNOWLEDGEMENT
We gratefully acknowledge the financial support from the National Science and
Engineering Research Council (NSERC) of Canada.
17
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19