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Rahman, Mohammad Mahbubur, Joardder, Mohammad Uzzal Hossain, &Karim, Azharul(2018)Non-destructive investigation of cellular level moisture distribution andmorphological changes during drying of a plant-based food material.Biosystems Engineering, 169, pp. 126-138.
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https://doi.org/10.1016/j.biosystemseng.2018.02.007
https://eprints.qut.edu.au/view/person/Rahman,_Mohammad_Mahbubur.htmlhttps://eprints.qut.edu.au/view/person/Joardder,_Mohammad.htmlhttps://eprints.qut.edu.au/view/person/Karim,_Azharul.htmlhttps://eprints.qut.edu.au/117264/https://doi.org/10.1016/j.biosystemseng.2018.02.007
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Non-destructive investigation of cellular level moisture distribution and morphological 1 changes during drying of a plant-based food material 2
M.M. Rahman1, Mohammad U.H. Joardder1, and M.A. Karim1* 3 4
1School of Chemistry, Physics and Mechanical Engineering, 5 Faculty of Science and Engineering 6
Queensland University of Technology, 7 Brisbane, Queensland, Australia 8
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*Author to whom correspondence should be addressed; 10
E-Mail: [email protected] 11
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Abstract 15
This study investigates the complex microstructural changes and cell-level water 16
transportation in plant-based food materials during drying, using X-ray micro-computed 17
tomography (X-ray µCT). The investigations were performed on apple tissue to uncover the 18
cellular level moisture distribution and the structural changes during convective drying at 19
50 °C, 60 °C, and 70 °C. Image analysis revealed that significant changes occurred in 20
moisture content, and cell and pore size distribution with drying time and temperature. The 21
moisture content determined using the X-ray µCT images was compared with that 22
determined by the electronic moisture analyser (EMA) and good agreement was found. The 23
results show a strong relationship between drying temperature, pore formation and 24
deformation of the food material. At high drying temperature, the pore formation increased, 25
which led to reduced shrinkage of the food material. The porosity of a sample of dried apple 26
increased by 35% as drying temperature increased from 50 °C to 70 °C. However, a 27
significant amount of cell rupture was observed during drying at the higher temperature. The 28
cellular level moisture distribution profile confirmed that a traceable amount of water was 29
still present in the centre cells of the tissue although the sample was deemed dried from the 30
bulk moisture analysis. The findings of this study substantially enhance our understanding of 31
instantaneous cellular level moisture distribution in a food sample over the time of drying. 32
Keywords: Food drying, cell rupture, porosity, transport, X-ray micro-tomography, water 33
distribution. 34
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1. Introduction 39
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The principle purpose of food drying is to remove moisture from the food material to increase 41
its shelf life while maintaining the quality of the product. Drying of plant-based food 42
materials is a complex process as it involves simultaneous heat and mass transfer and micro-43
level changes (Kumar et al., 2012; Rahman et al.,2016a). The microstructural changes 44
critically influence the overall transport process and the physical behaviour of food materials 45
(Rahman, Joardder, Khan, Nghia, & Karim, 2016). Moreover, moisture transport through the 46
intercellular spaces, and cells and cell walls of food materials occurs at the micro-level 47
(Aguilera, Chiralt, & Fito, 2003; Rahman, Joardder, Khan, Nghia, & Karim, 2016). 48
Therefore, it is essential to understand the micro-level transport mechanism and the 49
microstructural changes that take place during drying. 50
Plant-based food materials consist of cellular tissues, and the tissue consists of cells and 51
intercellular spaces (Joardder, Kumar, & Karim, 2015). A major component of plant-based 52
food materials is the water that is distributed in the microstructure. There are two types of 53
water in the food microstructure, which are classified based on their spatial locations. These 54
are free water (intercellular water) and bound water (intracellular water) (Khan, Wellard, 55
Nagy, Joardder, & Karim, 2017a). The bound water is located inside the cells whereas the 56
free water is located in the intercellular spaces. Research has shown that about 85% to 95% 57
of the water is bound in food materials, and the rest of the water remains in the intercellular 58
spaces and cell walls (Khan et al., 2016). The transport of bound and free water govern the 59
overall drying process (Rahman et al., 2016b), and therefore, it is crucial to understand the 60
water characteristics and their effect on the evolution of food microstructure in order to make 61
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an accurate prediction of energy requirement and the quality changes during food processing 62
especially drying. 63
The transport of water inside food tissue can take three pathways during drying, namely 64
symplastic, apoplastic and transcellular transport (Joardder, Kumar, & Karim, 2015). When 65
the sample has high moisture content, liquid water flows due to dominating capillary forces. 66
The bound water has lower diffusivity than the free water when the cells are intact (Fanta et 67
al., 2012). Therefore, the required energy for removing the bound water and free water from 68
the food microstructure is different. Bound water removal also affects the microstructure of 69
the food materials (Khan, Wellard, Nagy, Joardder, & Karim, 2017). Consequently, 70
knowledge of exact proportion of free and bound water is important and an appropriate non-71
destructive means of bound water measurement is crucial as destructive methods lead to 72
inaccurate measurements (Léonard et al. 2005). 73
There are several methods in the literature for determining cell-level water content in a fresh 74
food sample, including differential scanning calorimetry, bioelectrical impedance analysis, 75
dilatometry, thermogravimetric analysis, and nuclear magnetic resonance (NMR) (Khan & 76
Karim, 2017). The different types of water content inside food materials during drying were 77
determined by Khan et al. (2016a) using the NMR technique. However, the cell-wall 78
structure, cellular water, and intercellular water distribution cannot be identified clearly by 79
this method. Moreover, Khan et al.’s determination of various water contents relied on many 80
assumptions. To date, no research has been conducted to investigate the distribution of 81
cellular water (intracellular and intercellular water) during drying of food material. 82
It has been anticipated that the cell rupture takes place under certain drying conditions (Khan 83
et al., 2017; Rizzolo et al., 2014). Cell rupture depends on internal thermal stress that first 84
develops near the surface and gradually penetrates to the centre of the sample during 85
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convective drying (Khan et al., 2017). In other words, the entire food sample does not reach 86
breakdown temperature at the same time. Therefore it is a logical assumption that the cells 87
may collapse progressively from the surface to centre (Achanta & Okos, 1996; Askari, 88
Emam-Djomeh, & Mousavi, 2009; Gumeta-Chavez et al., 2011; Khan et al., 2017; Rahman 89
et al., 2015; Riva, Campolongo, Leva, Maestrelli, & Torreggiani, 2005; Yang, Di, Jiang, & 90
Zhao, 2010). Khan et al. (2017) reported that cells rupture at different stages of drying. 91
However, this progressive rupture was assumed, based on the pattern of the intercellular 92
water content. No clear evidence of cell rupture during drying was presented. 93
More complete microstructural information regarding the porosity and the cell rupture of 94
plant-based food is required to improve the physical quality of dried food. Although the 95
investigation of cellular level changes is critical to anticipate the overall shrinkage and 96
porosity of the food materials, only a limited number of studies have been found that dealt 97
with cellular level transport during drying (Joardder, Kumar, Brown, & Karim, 2015; 98
Karunasena et al., 2014; Khan et al., 2017). Most of the porosity measurement techniques 99
reported in the literature (e.g. solid displacement method) are destructive and invasive 100
(Joardder, Kumar, Brown, et al., 2015; Joardder, Kumar, & Karim, 2017). Therefore these 101
methods are not suitable to determine the instantaneous morphological changes during 102
drying. The limitations of destructive and invasive methods justify the importance of non-103
destructive and non-invasive methods. 104
Khan et al (2017) reported the NMR technique to be a suitable technique to uncover the 105
cellular level water distribution. However, this technique produces a large amount of noisy 106
data, and variations in cellular level water distribution cannot be readily identified. X-ray 107
µCT has proved to be valuable in the study of plants and plant-based food materials, 108
reflecting anatomical details of the entire tissue, especially the microstructure and the water 109
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distribution (Herremans et al.,2015; Mendoza et al.,2007). X-ray µCT is the most suitable 110
technique to address the elucidation of the cellular level transport mechanism during food 111
drying (Lim & Barigou, 2004; Rahman et al., 2016). 112
The earliest applications of computed tomography were in medicine. However, it has rapidly 113
become a very useful tool in physics (Wildenschild, Vaz, Rivers, Rikard & Christensen, 114
2002), biology (Momose, Takeda, Itai & Hirano, 1996), materials science (Salvo et al., 2003) 115
and multiscale engineering (Torre, Losada & Tarquis, 2016; Wood, Zerhouni, Hoford, 116
Hoffman & Mitzner, 1995). Recently, micro-tomography, based on micro-focus X-ray 117
sources, has become a relatively common tool for the characterisation of agricultural food 118
products (Donis-González, Guyer, Pease & Barthel, 2014; Schoeman, Williams, du Plessis & 119
Manley, 2016; van Dael et al., 2017) including apple (Almeida, Lancha, Pierre, Casalinho & 120
Perré, 2017; Diels et al., 2017; Si & Sankaran, 2016; Verboven et al., 2013), banana 121
(Madiouli et al., 2011), mango (Cantre, Herremans, Verboven, Ampofo-Asiama & Nicolaï, 122
2014), grains (Neethirajan, Karunakaran, Jayas & White, 2006; Zhu et al., 2012), kiwi 123
(Cantre et al., 2014), pears (Cantre et al., 2014; Muziri et al., 2016), carrot (Voda et al., 124
2012),and cucumbers (Donis-González, Guyer, Pease & Barthel, 2014). Today, commercially 125
available X-ray µCT allows non-destructive 3-D reconstruction of food materials at a spatial 126
resolution of a few micrometres (Verboven et al., 2008). 127
X-ray µCT was applied for the quantification of 3D pore space in fresh apple tissue 128
(Mendoza et al., 2007). Moreover, the X-ray µCT was used to characterise the multiscale gas 129
transport pathway in fresh apple and pome fruit, (Herremans et al., 2015; Verboven et al., 130
2008). Microstructural characterisation of mango ripening was also investigated by the X-ray 131
µCT (Cantre, Herremans, et al., 2014). 132
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However, the use of X-ray µCT for determining the micro-level changes during food drying 133
is limited in literature. This technique was used to determine the impact of freeze drying on 134
the microstructure of dried carrot, but the real-time moisture distribution inside the 135
microstructure during drying process was not investigated (Voda et al., 2012). Therefore, the 136
evolution of micro-level changes during drying could not be understood. Limited research 137
has been done regarding the non-invasive investigation of the cellular level transport 138
mechanism during drying of food materials (Almeida et al., 2017; Rathnayaka, Karunasena, 139
Senadeera, & Gu, 2017). Moreover, much of the research failed to elucidate the role of food 140
microstructure changes on the drying kinetics (Schoeman et al., 2016). Therefore, there is a 141
critical need to use X-ray µCT to investigate cellular level phenomena during drying of plant-142
based food materials. 143
The primary objective of this work is to investigate experimentally the instantaneous 144
morphological changes, real-time cellular level moisture distribution, and cell and pore size 145
distribution during drying of plant-based food materials. 146
2. Materials and methods 147 148
2.1 Sample preparation and the drying experiment 149
Granny Smith apple was used for the experiments. The fresh apples were collected from the 150
local market and stored in a refrigerator at 4 °C to keep them fresh before the drying 151
experiment. Prior to the drying test, the samples were taken from the refrigerator and kept at 152
the room temperature for an hour to achieve thermal stability. The samples were then cut as 153
cylindrical slices from the middle parenchyma region (2 cm to 3 cm under the peel) of the 154
apples with the dimension of 1 mm thickness and 5 mm diameter. For each drying 155
experiment, six samples were used, and each sample was taken from the same region of six 156
different Granny Smith apples. In order to investigate the influence of sample size on the 157
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morphological changes during drying, a larger sample with the dimension of 20 mm diameter 158
and 10 mm thickness was also prepared from the middle parenchyma region. 159
160
The dryer was run for 30 min before the experiment, to allow the system to reach steady 161
state. The drying experiments were carried out in a laboratory-scale temperature-controlled 162
cabinet-type convective dryer. The dryer had an electric heater and a fan to produce 163
controlled perpendicular hot air flow across the samples throughout the experiment. The 164
temperature of the dryer could be adjusted within the temperature range 30 °C to 70 °C. To 165
ensure uniform heat transfer, the samples were placed symmetrically on the same tray in 166
close proximity to the central axis and air inlet vent of the equipment. The samples were 167
placed in the tray only after the dryer reached a steady state condition. The drying 168
experiments performed were based on the American Society of Agricultural and Biological 169
Engineers (ASABE S448.1) standard at three different temperatures 50 °C, 60 °C and 70 °C. 170
This range of temperatures is widely used in the drying industries for the maximum retention 171
of quality attributes (Tsotsas & Mujumdar., 2011). During each experiment, air velocity was 172
0.7 m s-1 and relative humidity ranged between 60% and 65%. The samples were taken out 173
from the dryer every 30 minutes for X-ray µCT experiments. Before placing them into the X-174
ray µCT, the samples were kept in a desiccator to avoid the natural rehydration from the 175
ambient humidity. The samples were then scanned using a Scanco µCT40 high-resolution 176
desktop µ-CT system (Scanco Medical, Brüttisellen, Switzerland) with a resolution of 6 µm. 177
After scanning, the samples were placed back into the dryer, and the scanned images were 178
saved for further investigation. The moisture content of the sample at the different stages of 179
drying was measured by EMA (KERN_MLA, Germany). The moisture analyser was 180
calibrated by the AOAC method (Official method 1995) (Ahn, Kong, & Kim, 2014). The 181
initial moisture content of the fresh apple sample was determined to be 90% wet basis. 182
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2.2 X-ray micro-tomography 183
The Scanco µCT-40 was used in this study to investigate the micro-level transport 184
phenomena. The moisture content obtained from the X-ray µCT method was compared with 185
the results from the moisture analyser to justify the applicability of the approach. X-ray µCT 186
uses x-rays to create 2D cross-sections of a physical object that are then used to create a 187
virtual model (3D model) without destroying the original object. It is able to scan the entire 188
sample to obtain micro-level information such as moisture distribution, cells, and pore size 189
distribution without the need of serial cuts or chemical treatment. Therefore, the same sample 190
can be analysed at different stages of the drying process. The scanning was operated at 55 191
kV, and the images were taken through 0° to 360° of rotation. The detector of the X-ray 192
tomography is a 2D camera with the resolution of 4069×4069 pixels and spatial resolution of 193
6µm. The samples were rotated horizontally between 0° to 360° angle to get the 2D scans at 194
different vertical positions. The minimum distance between two scans is 6µm. The images of 195
the middle part of the sample were considered for the analysis. The reconstruction of the 2D 196
images was performed with the built in software packages that uses the back-projection 197
algorithm. The 3D analysis can also be performed from the 2D cross section image stacks of 198
the sample by the Itanium2 based ‘Open VMS’ software package supplied with the Scanco 199
µCT-40 system. However, 2D analysis was performed in this study to get a clear observation 200
of the cross section of the sample. 201
2.4 Image processing 202
The greyscale images obtained from the X-ray µCT were transferred to a MATLAB image 203
processing environment for further processing. Adjustment of the greyscale image contrast 204
was performed by the “imadjust” function of MATLAB. The image processing involved 205
noise elimination and segmentation. The steps involved in the proposed image processing 206
method are presented in Figure 1. 207
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208
Figure 1. can be inserted here 209
210
The noise elimination was performed by intensity thresholding and filtering. Segmentation 211
was performed after noise elimination to characterise solid materials in the microscopic 212
images. For this purpose, the watershed algorithm was used (Ng, Ong, Foong Goh, & 213
Nowinski, 2006). It was found that the cell wall exhibited a higher intensity value compared 214
to the water-filled cells. The difference between intracellular water and the intercellular water 215
was classified by the manual segmentation process. For the improvement of the classification, 216
a global threshold value was defined based on the intensity of the images. The cells and the 217
intercellular spaces were identified from the reconstructed greyscale images. The 218
classification of the cell wall, water-filled cells and intercellular spaces was performed based 219
on the intensity variation. 220
2.4.1 Measurement of cellular level moisture content 221
Image processing using MATLAB to determine moisture content was performed by creating 222
the region of interest in each part of the scanned image. To determine the moisture content 223
from the micro-tomographic images, the grey level intensity of each section of the image was 224
analysed. The process of determining the moisture content from the tomographic images is 225
available in the literature (Léonard, Blacher, Marchot, Pirard, & Crine, 2005) and the 226
following equation is commonly used: 227
Moisture Content =(Grey level)Dry solid−(Grey level)wet solid
(Grey level)Dry solid−(Grey level)water )3( 228
In equation (3) the (Grey level)Dry solid represents the grey level of cell wall, 229
(Grey level)wet solid represents the intracellular water and (Grey level)water represents the 230
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intercellular water. The intracellular and the intercellular water contents were obtained from 231
the X-ray µCT images by selecting the region of interest (ROI) manually and applying 232
equation (3). Each of the ROI was selected and analysed manually. The selected ROI in the 233
cellular region provides the information of intracellular water and the selected ROI in the 234
intercellular region provides the information of the intercellular water. The proportion of 235
intracellular water and intercellular water can be expressed by the following relationships 236
Proportion of Intracellular water = Intracellular water Intracellular water+Intercellular water
× 100 (4) 237
Proportion of Intercellular water = Intercellular water Intracellular water+Intercellular water
× 100 (5) 238
2.4.2 Measurement of equivalent cell diameter 239
The equivalent diameter of each region was calculated using the following relationship: 240
Equivalent diameter =�4×𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝜋𝜋
(6) 241
The areas of the cells and intercellular spaces were obtained from the pixels in the X-ray µCT 242 image. 243
2.4.3 Porosity measurement 244
The porosity of the samples at different stages of drying was determined from the X-ray µCT 245
data. The porosity was calculated using the following relationship (Joardder, Karim, Kumar, 246
& Brown, 2015): 247
Porosity = total volume of intercellular spaceTotal volume of the sample
(7) 248
2.4.4 Measurement of cell rupture 249
Digital image correlation (DIC) was used to measure the amount of cell rupture during 250
drying. The DIC technique compares a series of digital photographs at different stages of 251
drying. This technique directly shows the cellular level evolution of food samples to sub-252
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pixel accuracy. The DIC analysis was performed in MATLAB (MATLAB 2015b) based on 253
the algorithm developed by Pan et al., (2009). The DIC was performed by registering two X-254
ray micro-tomographic images of the sample during drying process. One image was taken 255
from the fresh sample which was considered as reference image and the other images were 256
taken at the different stages of drying for comparing with the reference image. The pixel and 257
the intensity of the images were kept consistent by adjusting the grey level histogram for the 258
effective performance of the DIC process. The ruptures of the cellular structure were 259
evaluated based on the image morphology analysis concept adopted from Lecompte et al. 260
(2006). The morphology analysis is an image processing technique which considers the shape 261
of the elements in the images. The shape of the cells and the intercellular spaces were found 262
from the pixel of the image. The morphological operation was performed by estimating the 263
size and the shape of the corresponding cell or intercellular space in MATLAB image 264
processing toolbox. The detail information regarding the calculation of the structural 265
morphology can be found in author’s previous publication (Rahman et al. 2018). The 266
evaluated ruptures from different sample were compared for the error analysis. 267
2.5 Statistical analysis 268
The experiments were repeated six times for each drying condition. The results were 269
expressed as mean and standard deviation (Swasdisevi, Devahastin, Sa-Adchom, & 270
Soponronnarit, 2009) corresponding to the moisture content and the equivalent diameter of 271
the cells. Moisture profile measured by the moisture analyser and X-ray µ-CT was compared 272
by the coefficient of determination (R2) and standard error of estimation (SEE) analysis. The 273
coefficient of determination (R2) was calculated using the following standard equation: 274
𝑅𝑅2 = [𝑛𝑛 ∑𝑋𝑋𝑋𝑋−(∑𝑋𝑋)(∑𝑋𝑋)]2
[𝑛𝑛 ∑𝑋𝑋2−(∑𝑋𝑋)2][𝑛𝑛 ∑𝑋𝑋2−(𝑋𝑋)2] (6) 275
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where 𝑅𝑅2 is the coefficient of determination, X is the moisture content determined by the 276
moisture analyser (dry basis), and Y is the moisture content determined by the X-ray µ-CT. 277
The SEE was determined using the following equation: 278
𝑆𝑆𝑆𝑆𝑆𝑆 = �∑(𝑊𝑊−𝑊𝑊� )2
𝑁𝑁−2 (7) 279
where W is the moisture content data, 𝑊𝑊� is the average value of the moisture content data, N 280
is the number of data points. 281
3. Results and discussions 282
3.1 Moisture distribution in fresh sample 283
A tomographic image of the fresh apple slice showing the water distribution is presented in 284
Figure 2. In the figure, the darker colour represents the lower intensity, while the lighter 285
colour represents the high intensity of the µ-CT image. The intensity difference between the 286
intracellular and intercellular water is significant as the concentration of intracellular water is 287
higher than the intercellular water. The intensity difference between the intracellular water 288
and the cell wall is also substantial as the cell walls are made of solid materials. Therefore, 289
the presence of cell walls, intracellular water, and intercellular water can be determined from 290
the X-ray µCT technique. It can be determined from Figure 2 that there was little water (5–291
7%) present in the intercellular space, while about 90% to 95% of the water was inside the 292
cells surrounded by the cell membrane and wall. The greyscale bar on the left side of the 293
image represents the concentration of moisture content throughout the sample. When the 294
greyscale value is 1, it is considered that there is strongly bound water entrapped in the cell 295
wall. On the other hand, the zero-greyscale value represents the void section inside the tissue. 296
It is interesting to note that the moisture distribution in fresh apple tissue was not uniform 297
throughout the whole sample as some pore space was evident in the fresh sample. 298
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Figure 2 can be inserted here 300
301
3.2 Changes in moisture distribution during drying 302 303
A relationship between the bulk moisture content and the cellular level moisture distribution 304
during drying in an apple sample at 60 °C is presented in Figure 3. It is clear from the figure 305
that the reduction of bulk moisture is accompanied by the reduction of intracellular water. 306
307
Figure 3 can be inserted here 308
309
In the initial drying stage, most of the water remains inside the cells. In the literature, the 310
intercellular water is considered as loosely bound water, and therefore it is assumed that the 311
energy requirement for removing intercellular water is low (Khan et al., 2017b; Rahman et 312
al., 2016). The intercellular water migration leads to the fast drying of the intercellular region 313
in the apple sample. As drying progresses, the concentration of intracellular water also 314
decreases. In the first phase of drying the reduction of overall moisture content is significant. 315
In this phase, the transport of cellular water occurs through the cell membrane and cell wall. 316
As drying continues, heat is transferred from the peripheral cells to the internal cells and 317
creates the pressure gradient between intracellular and intercellular spaces (Khan et al., 318
2017b). This phenomenon leads to rupture of the cell membranes of the apple tissue. Rupture 319
of cell membranes facilitates migration of cellular water (both intracellular and intercellular). 320
A clear representation (with larger image) of the cellular level water distribution and the cell 321
rupture at different stages of drying at 60°C is presented in Figure 4. Analysis of the cell 322
rupture is presented in section 3.4. In the last phase of drying (200–350 min), the centre cells 323
contain more intracellular water than intercellular water. Intracellular water is removed in the 324
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last stages of drying (Khan et al., 2017b). Most of the energy required for the drying process 325
is for the removal of the intracellular water. 326
Figure 4 can be inserted here 327
328
The overall bulk moisture contents during drying at 50 °C, 60 °C, and 70 °C were calculated 329
from the tomographic images using equation (3). For the validation of the proposed method, 330
the moisture content determined from the tomographic images was compared with the results 331
obtained by the moisture analyser. The comparison is presented in Figure 5. A good 332
agreement has been found between the moisture content determined from the tomographic 333
images and the EMA. The coefficient of determination (R2) and the SEE were 0.998 and 334
0.001 respectively. 335
336
Figure 5 can be inserted here 337
Figure 6 shows the evolution of intercellular and intracellular water in the apple sample 338
during drying at 50 °C, 60 °C and 70 °C temperatures. It is clear from the figure that the 339
drying temperature has a major influence on the transport of intracellular water. At the lower 340
drying temperature (50 °C) the intracellular water decreased slowly, as shown in Figure 6a. 341
This is because the cell membrane remains intact during the process and it is called the 342
intracellular transport process (Halder et al. 2011). The loss of intracellular water was 343
significant in 60 °C and 70 °C temperature as shown in Figure 6b and c. This is because 344
significant cellular rupture occurs at higher temperatures, which facilitates the rapid 345
migration of the intracellular water. It was found from the literature that when the 346
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temperature is above 50 °C, the cell membrane starts to break (Khan et al. 2017; Halder et al. 347
2011). 348
349
Figure 6 can be inserted here 350
3.3 Morphological changes 351
The structural change of food material is the result of cell rupture and shrinkage of the sample 352
during the drying period when significant loss of water takes place (Devahastin & Niamnuy, 353
2010; Ramos, Branda, & Silva, 2003). There is a fine difference between cell rupture and 354
shrinkage of the sample. Cell rupture and shrinkage of the sample are directly related to the 355
cell and the pore size distribution. The cell and pore size distribution inside the sample at 356
different temperatures and drying times is illustrated in Figures 7–9. In these figures, blue 357
bars represent equivalent cell diameter, and the brown bars represent the equivalent diameter 358
of the intercellular spaces. The equivalent diameter of cells and intercellular spaces were 359
obtained from the image analysis by using equation (6). The highest values of equivalent 360
diameter for cell and intercellular spaces were around 310 µm. Therefore, the size 361
distribution of cells and intercellular spaces is presented between 0 µm and 320 µm with an 362
equal interval of 20 µm in order to investigate the evolution of cell and intercellular spaces 363
during drying. In Figures 7-9, the x-axis represents the equivalent diameter of cells and 364
intercellular space and the y-axis represents the percentage of the cells and intercellular 365
spaces fall within a certain range. 366
The size distribution of cells and the intercellular spaces during drying at 60 °C is presented 367
in Figure 7. In the fresh sample, the cell size was larger than the pore or intercellular space, as 368
shown in Figure 7a. It can be seen in the figure that most of the cells had equivalent 369
diameters in between 181 µm and 220 µm while the equivalent diameter of the intercellular 370
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space mostly varied from 50 µm to 220 µm. It was found from the literature that food 371
materials shrink without cell collapse in the first phase of the drying process. As the drying 372
progressed, the cell size reduced slowly while the pore size distribution changed rapidly 373
(Figure 7b). The diameter of most of the cells remained in between 120 µm and 180 µm. 374
According to the literature, the water migration process in this stage is mainly the free water 375
removal (Khan et al. 2017). During the drying process, negative pressure is created inside the 376
cells due to the removal of water, which is the major reason behind the cellular level 377
deformation (Joardder, Karim, Kumar, & Brown, 2016). Owing to ongoing moisture 378
migration, the collapse of cells and intercellular spaces increased in the later stages of drying. 379
At this stage, the equivalent diameter of most of the intercellular spaces was higher than 100 380
µm and the majority were in between 120 µm and 140 µm. The pore size distribution was 381
greater than the cell size distributions at the later phase of the drying process shown in Figure 382
7c and d. 383
Figure 7 can be inserted here 384
The temperature has a great effect on the size distribution of cells and the intercellular spaces 385
during drying. Figure 8 shows the size distribution of cells and intercellular spaces at 386
different stages of drying at 50 °C. When the apple was dried at a lower temperature (50 °C), 387
there was less cell collapse but more shrinkage of the tissue due to the prolonged drying time. 388
After 60 min of drying, the equivalent diameter of the cells was in between to 120 µm and 389
140 µm. It is clear from Figure 8a that the equivalent diameter of the intercellular spaces did 390
not increase significantly in this phase of drying. At the later phase of the drying process 391
(Figure 8b and c), the equivalent diameter of most of the cells dropped to 100 µm. On the 392
other hand, the diameter for most of the intercellular spaces did not increase over 150 µm. 393
Figure 8 can be inserted here 394
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Figure 9 shows the size distribution of cells and intercellular spaces at different phases of 395
drying at 70 °C. As shown in Figure 9a, after 60 min of drying time the diameter of 35% of 396
the cells reduced to 120 µm, but the diameter of 38% of the intercellular spaces remained 397
between 120 µm and 150 µm. As drying progressed at high temperature, the size distribution 398
of cells and intercellular spaces also changed significantly. Figure 9 b and c represent the 399
morphological changes in the apple tissue in the later part of drying (200 min and 300 min 400
respectively). The size of the intercellular space was larger than the cell size. At this phase of 401
drying the diameter of more than 40% of the cells dropped below 100 µm. On the other hand, 402
the diameter of more than 60% intercellular space increased to over 150 µm. The results 403
imply that drying at low temperature leads to smaller pore size while drying at high 404
temperature leads to larger pore size. The comparative study of the porosity evolution in the 405
apple sample at different drying temperatures is discussed in section 3.5. 406
Figure 9 can be inserted here 407
3.4 Analysis of the cell rupture 408
As shown in this study, the rupture of the cellular structure takes place during drying. Drying 409
temperature significantly contributes to the cell rupture. The drying parameters like air flow 410
and humidity usually play a less significant role in the dehydration process (Kumar et al. 411
2015). Figure 10 shows the percentage of cell rupture at different temperatures and different 412
stages of drying. It is clear from the figure that cell rupture increased significantly with 413
temperature. After drying at a temperature of 50 °C, around 22% of the cells of the dried 414
sample had ruptured, while at 60 °C and 70 °C the cell rupture levels were 70% and 82% 415
respectively. 416
Figure 10 can be inserted here 417
18
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The rupture of the cellular structure at different stages of drying at 60 °C temperature is 418
clearly visible in Figure 4. Figure 11 shows X-ray µ CT image of the larger sample of apple 419
microstructure dried at 60 °C. It is clear from the analysis that cell rupture is mainly assisted 420
by the temperature. It was found that when the experiment was conducted with the larger 421
sample at 60 °C, the drying time extended up to 540 min. Therefore, it takes more time for 422
cell rupture to occur during drying. However, the cell rupture followed similar trends in 423
breaking sequence during the high-temperature drying process. A significant amount of cell 424
rupture was still observed in the micro-tomographic image of the dried apple sample. 425
Figure 11 can be inserted here 426
427
3.5 Porosity 428
The porosity of the samples was calculated from the images using equation (7). The porosity 429
of the plant-based food materials also showed an interesting relationship between moisture 430
content and the drying temperature. Figure 12 shows the changes of porosity of apple sample 431
at different drying temperature against the moisture content. It is clear from the figure that 432
drying the food material at high temperature led to higher porosity. 433
Figure 12 can be inserted here 434
It is shown in Figure 12 that a decreasing trend of porosity was found at the beginning of 435
drying and just before an increasing trend started at a moisture content of 0.7. After that, 436
porosity kept increasing steadily with moisture content until the end of the drying process. 437
The drying temperature influenced the overall structure of the food materials by contributing 438
to the pore formation inside the sample. From the figure, it can be seen that the porosity 439
19
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increased by 35% with an increase of drying air temperature from 50 °C to 70 °C. The 440
mechanism of the pore formation is discussed by the authors in their previous work (Joardder 441
et al., 2016). This higher porosity in the case of drying at higher temperature can be referred 442
to a shorter time required for drying. 443
4. Conclusion 444
This paper presents the analysis of cellular level water distribution, morphological changes, 445
and cell and pore size distribution of apple samples during drying using a non-destructive X-446
ray µCT method. It has been found that the cell and the pore size distribution of the food 447
material change significantly over the drying time. The investigation also showed that the 448
transport of water inside the cellular tissue of food material is governed by the drying 449
temperature. At the first stage of drying, most of the water is bound water while in the later 450
stage of drying most of the water becomes ‘free water’ as cells are ruptured, and intracellular 451
water migrates to intercellular spaces. Another striking finding of this study is that high-452
temperature drying leads to less shrinkage despite a significant amount of cell rupture at a 453
higher temperature. Other process parameters like the air velocity and the air humidity have a 454
lower effect (compared to temperature) on cell rupture as the drying process is not 455
significantly influenced by these two parameters (Kumar et al., 2015). This study also found 456
that porosity is influenced by the drying temperature. The porosity of the dried apple 457
increased by 35% with the increase of temperature from 50 °C to 70 °C. The findings of this 458
study will enable future researchers to better understand the relationship between drying 459
conditions and micro-level transport phenomena. In addition, the findings will assist food 460
engineers in the development and validation of an accurate transport model, which will lead 461
to the design of an energy-efficient food drying system. 462
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Acknowledgement 463
This research is supported by Queensland Government Advanced Queensland Fellowship. 464
The authors acknowledge the facilities and the technical assistance of the Institute of Health 465
and Biomedical Innovation. The authors also gratefully acknowledge the support of Dr. 466
Marie-Luise Wille. 467
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Abstract1. Introduction2. Materials and methods2.1 Sample preparation and the drying experiment2.2 X-ray micro-tomography2.4 Image processing2.4.1 Measurement of cellular level moisture content2.4.2 Measurement of equivalent cell diameter2.4.3 Porosity measurement2.4.4 Measurement of cell rupture2.5 Statistical analysis
3. Results and discussions3.1 Moisture distribution in fresh sample3.2 Changes in moisture distribution during drying3.3 Morphological changes3.4 Analysis of the cell rupture3.5 Porosity
4. ConclusionAcknowledgementReferences