Journal of Food Engineering 214 (2017) 117e128

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Journal of Food Engineering

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Microstructure investigation and its effects on moisture sorption in

fried potato chips*
Jun Yang a, *, Aaron Martin a, Scott Richardson a, Chih-Hsien Wu b
a
Analytical Sciences, PepsiCo Global R&D, 7701 Legacy Drive, Plano, TX 75024, USA
b
Global Statistics & Data Modeling, PepsiCo Global R&D, 7701 Legacy Drive, Plano, TX 75024, USA

a r t i c l e i n f o a b s t r a c t

Article history: It is important to understand the influence of processing conditions to design a desirable food product.
Received 26 January 2017 The microstructure and water sorption capacity of three types of fried potato chips were evaluated in
Received in revised form order to gain an understanding of how the different processing conditions impacted their structures and
13 May 2017
further, their textures and shelf life. Pore structures were quantified and analyzed using both the
Accepted 27 June 2017
Available online 28 June 2017
capillary penetration technique of a mercury porosimeter and the imaging technique of X-ray computed
tomography (mCT). Additionally, the water vapor sorption isotherm was quantified using a Pro Umid
SPSx-1m system. The results indicated that ridged potato chips (RPC) showed the highest porosity
Keywords:
Fried potato chips
(50.78 ± 3.02%), followed by flat potato chips (FPC) (41.15 ± 3.56%), and batch cooked potato chips (BCPC)
Microstructure (32.58 ± 4.21%). A similar trend was exhibited in the data obtained from X-ray mCT. The solids distri-
X-ray computed tomography bution in RPC, FPC, and BCPC was 21.56 ± 7.97%, 24.87 ± 5.83%, and 34.28 ± 9.49%, respectively, deter-
Mercury porosimeter mined by mCT. mCT cross-section images displayed a highly porous microstructure in FPC, while RPC
Moisture sorption isotherm appeared to have thicker walls and larger cells than the others. The data suggested that the critical water
activity (aw) of the three types of potato chips ranged from 0.70 to 0.85. At higher aw (above 0.85), RPC
displayed the highest moisture absorption capacity, followed by FPC, and BCPC. The results also showed
that a higher percentage of porosity is followed by higher moisture content in the potato chips. The
findings propose that water vapor sorption of the three types of potato chip was governed by the Flory-
Huggins model. In addition, the oil significantly blocked water sorption in the samples (p < 0.05).
© 2017 Elsevier Ltd. All rights reserved.

1. Introduction gelatinization and retrogradation of starch (Alvarez et al., 2001;

The potato (Solanum tuberosum L.) is an important vegetable
widely grown around the world. Frying, as one of the oldest unit
operations, is commonly applied in potato processing to produce
desirable products such as potato chips. The textural changes dur-
ing thermal processing of potato tubers have been associated with
the breakdown of the cell wall and middle lamellae structural
components. For example, at cellular level frying induces cell sep-
aration, shrinkage, wrinkling, and cell wall convolution around
dehydrated gelatinized starch without cell wall rupture (Costa
et al., 2001). Additionally, the texture is transformed by the
*
All authors are employees of PepsiCo Inc. The views expressed in this manu-
script are those of the authors and do not necessarily reflect the position or policy
of PepsiCo Inc.
* Corresponding author.
E-mail address: Jun.Yang@pepsico.com (J. Yang).
Ormerod et al., 2002), as moisture evaporates and oil penetrates
the structure. During the above processes, the solid matrix and
porosity of potato chips are formed. Meanwhile, oil fills the voids
and covers the surface. Therefore, physiochemical properties
(texture and color), structural properties (porosity and roughness),
oil and water content have all been designed by the processing
conditions. Together, each of these properties has a significant ef-
fect on the quality of potato chips. Texture is considered as one of
the most important quality attributes of a potato chip experienced
by consumers. Crispy and crunchy textures are desirable charac-
teristics, which contribute to enjoyment of potato chips. Those
properties are associated with porosity, solids, and oil in the
finished products. The microstructure of potato chips is generally
quantified in terms of porosity, average cell size, cell wall thickness,
and cell size distribution. The ratio of cell wall thickness over the
cell size is an important indicator in controlling the crispiness
(Dogan and Kokini, 2007).
X-ray mCT is a powerful noninvasive and nondestructive imaging

http://dx.doi.org/10.1016/j.jfoodeng.2017.06.034
0260-8774/© 2017 Elsevier Ltd. All rights reserved.
118 J. Yang et al. / Journal of Food Engineering 214 (2017) 117e128
technique allowing for high-resolution 3-D visualization, quantifi-
cation and characterization of the internal structure of a sample
based on local variation of the X-ray attenuation coefficient. This
technique has been used to obtain reliable microstructural infor-
mation of many porous products which have undergone different
processing conditions (van Dalen et al., 2007; Zhu et al., 2012).
Samples which have been analyzed with X-ray mCT include both
raw ingredients and finished products, such as vegetables (van
Dalen et al., 2013), apple (Ho et al., 2014), corn (Takhar and
Zhang, 2009), cereal and crackers (van Dalen et al., 2007), and
bread (Lape et al., 2008). As an imaging technique, it can deliver
significant microstructural details and provide an in-depth inves-
tigation of the internal structure in products through capturing
meaningful quantitative data including total volume of interest
(VOI) and surface, object surface/volume ratio, structure thickness,
number/volume/surface of closed pores, total porosity (%), and
connectivity. For instance, mCT has given reliable information about
the total pore volume and pore size distribution in the samples,
having quantified the pore space of apple tissue (Herremans et al.,
2013), examined the effect of far-infrared radiation assisted drying
on microstructure of banana slices (Le onard et al., 2008), and
characterized the tissue of air-dried apple rings (Rizzolo et al.,
2014).
As a non-invasive technique, mCT scanning allows examination
of microstructures, and further understand the relationship be-
tween processing and potato chip attributes. High-resolution X-ray
mCT can visualize features in the interior of opaque solid objects,
resolve details as small as a few microns in size, and acquire digital
information on their 3-D geometries and properties. It is as simple
as passing X-rays through the object and obtaining information
with a detector on the other side. The X-ray source and the detector
are interconnected and the object is rotated 180
during the
scanning period. Later the data are assembled and integrated to
provide a cross sectional image (tomogram). The image(s) can be
analyzed for various features. It generates 2-D representations of a
slice of an object based on material density. Slices from a scanned
object can be stacked to produce a 3-D reconstruction. The result-
ing slice is made up of voxels (3-D pixels). Each voxel is assigned a
CT (grey) value derived from a linear attenuation coefficient (i.e.
density) of the material(s) being scanned. Microstructure including
the size and diameter of pores and solids, forms the fundamental
texture of potato chips.
It is well known that moisture migration in fried snacks plays a
critical role in the loss of firmness and crispiness, which further
affects the shelf life of products. Although moisture diffusivity
calculated by solving Fick's second law of diffusion is well corre-
lated to the temperature and moisture content of a product,
microstructure and chemical composition also have an important
effect on moisture migration (Gueven and Hicsasmaz, 2013). It is
difficult to characterize moisture migration in potato chips, which
is the consequence of a number of coexisting moisture transport
mechanisms, as well as the complexity of the product microstruc-
ture (i.e. porosity and solids), and compositions such as interaction
of water with oil and salt (Roca et al., 2006). A previous study
revealed that an increase in porosity accompanied by an open pore
structure is believed to increase moisture diffusivity to a great
extent (Baik and Marcotte, 2003). The moisture sorption isotherm
is useful in predicting potential changes in product stability,
determination of ideal storage conditions, packaging selection, and
providing valuable information about changes related to the ther-
modynamics of the system. Many empirical and semi-empirical
models, including GAB, Halsey, BET, Oswin, Henderson, Peleg,
Caurie, and Lewicki (Rao et al., 2006; Basu et al., 2006), have been
proposed to describe the moisture sorption characteristics of foods.
Moisture sorption isotherms of potato chips reflect the integrated
hygroscopic properties of the individual components and micro-
structure including pore size and pore distribution. Therefore, any
modifications in both microstructure and chemical composition of
the sample may influence its sorption equilibrium properties.
Porosity, solids, and oil in potato chips are of great interest in
product design, selection of processing condition, organoleptic and
texture properties. Recently, Alam and Takhar (2016) have used X-
ray mCT technique to characterize microstructural changes in potato
disks during frying. mCT was utilized for 3-D imaging of micro-
structure of porous potato disks. The 3D rendering of the images
yielded information on porosity, pore size distribution, tortuosity,
and spatial location of oil droplets. It was concluded that mCT
technique can serve as an effective tool for elucidating micro-
structure of fried foods. Ridged potato chips (RPC) and flat potato
chips (FPC) are dehydrated via movable and continuous frying,
using a conveyer-belt-like continuous process, while batch cooked
potato chips (BCPC) are dehydrated using a stationary frying, and
made in batches. Porosity and pore size distribution in these
products are critical microstructural properties required in process
optimization, product development, and shelf life stability. There-
fore, it is important to fundamentally understand and apply
advanced analytical techniques to characterize the microstructure
of potato chips in order to explore its relationship with different
processing conditions and shelf life. Scanty information is available
in the literature regarding the evaluation of microstructure in po-
tato chips by both the capillary penetration technique of mercury
porosimeter and the imaging technique of X-ray mCT. Therefore, the
objective of the present study was to characterize pore properties
(pore size and distribution) by mercury porosimeter, and quantify
pores and solids using X-ray mCT in three types of potato chips. The
water vapor sorption isotherm was evaluated using a controlled
atmosphere microbalance in the SPSx-1m system. Furthermore, the
relationship between relative humidity (RH), porosity, solids, oil
and water sorption was statistically assessed.
2. Materials and methods
2.1. Sample
Three types of potato chips named flat potato chips (FPC), batch
cooked potato chips (BCPC), and ridged potato chips (RPC) were
purchased in the local market. These samples were selected based
on having the same potato variety and frying oil, but with different
slice thickness (before frying), and processing conditions.
2.2. Moisture measurement
The moisture content of the potato chips was determined using
a moisture meter (model TGA-701, Leco Corporation, St. Joseph, MI,
USA). Generally, samples were collected and stored in air-tight jars
until they were ready to be tested. Each cup was loaded with 2e4 g
of the sample before being put into the carousel and set at 103
C.
2.3. Color determination
The color of the potato chips was determined using a HunterLab
Model D25LT spectrocolorimeter with the CIE L*, a* and b* color
scale (HunterLab Inc., Reston, VA, USA). In this coordinate system,
the L* value is a measurement of lightness, ranging from 0 (dark-
ness) to 100 (brightness). The a* value ranges from 100 (green-
ness) to þ100 (redness). Lastly, the b* value ranges from 100
(blueness) to þ100 (yellowness). The ground samples were packed
evenly and smoothly up to the lid of three small petri dishes before
being placed in the spectrocolorimeter one at a time. The L*, a* and
b* values were recorded each time.
 J. Yang et al. / Journal of Food Engineering 214 (2017) 117e128
2.4. Salt quantification
Salt content in each single potato chip was quantified using the
DL53 titrator (Mettler-Toledo, LLC, Columbus, OH).
2.5. Oil determination
Soxhlet Extraction by Buchi E-816 (BUCHI Corporation, New
Castle, DE) was used to determine the percentage of non-volatile oil
in the samples.
2.6. Absolute density measurement
The density of the potato chips was quantified using the AccuPyc
II 1340 Automatic Gas Pycnometer (Micromeritics, Norcross, GA)
which determines the true volume of samples with an irregular
shape.
2.7. Mercury intrusion evaluation analysis of pore volume and size
in potato chips
The porosity of the potato chips was determined and analyzed
by AutoPore™ IV Series Automated Mercury Porosimeter (Micro-
meritics Instrument Corporation, Norcross, GA, USA). The mercury
porosimetry analysis technique is based on the intrusion of mer-
cury into a porous structure under stringently controlled pressures.
It provides a calculation of sample properties including pore size
distribution, total pore volume, total pore surface area, median pore
diameter, and sample densities. The Porosimeter can determine a
broad pore size distribution (0.003e360 mm). In this study, the 942-
10 High-resolution macropore analysis ISO 15901-1 method was
applied. Briefly, the pore size was analyzed from 900 to 4 mm
(macropore size). Pressure ranged from 0.25 to 45 psia. Initial
evacuating speed was set at 5.0 psia/min. Evacuation was targeted
at 50 mm mercury (Hg). Both mercury advancing and receding
contact angles were 130.000
. Mercury surface tension was
485.000 dyn/cm. Mercury density was 13.5462 g/mL. Filling pres-
sure was 0.200 psia.
2.8. Microstructural characterization by X-ray microtomography
and image analysis
2.8.1. Scanning and reconstruction
The potato chip samples were scanned using a SkyScan 1172
high resolution X-ray mCT system (Desktop X-ray microtomograph,
SkyScan N.V., Aartselaar, Belgium) consisting of an X-ray tube, an X-
ray detector, and a charge coupled device (CCD) camera. Experi-
mental conditions were optimized to allow for high quality radio-
graphic projection images considering contrast, resolution and
manageable scanning times. A sample was placed vertically in a
polystyrene holder, which is almost transparent to X-rays. The X-
ray source and detector were fixed, while the sample was rotated
during the measurement. The cone beam source was set at 40 kV/
250 mA, suitable for scanning hard materials to acquire optimum
contrast of void (porosity) and matter (solid). The images were
captured using a 16-bit, cooled CCD camera (8000  8000 pixels).
Samples were scanned at a magnification of 2000  1336 pixels.
The distance between object and camera was adjusted to produce
images with a pixel size of 6.5 mm. The exposure time of camera was
set as 215.0 ms. X-ray images were obtained for every 0.2
of
rotation for a total of 1226 shadow images (radiographs)/sample.
The actual obtained pixel size was 5.93874 mm. The total scan time
was between 60 and 90 min/sample.
Upon completion of scanning, the X-ray shadow projections of
the 3-D object were digitized as 2048  2048 pixel images.
119
Additionally, they were processed to obtain reconstructed cross-
section images using a mathematical algorithm based on the
filtered back projection procedure implemented in the NRecon
reconstruction software (V1.6.10.4). This software combines the
images, graphically, into a 3-D object from 2-D cross-sectional
images. Before the reconstruction process, the cross section (CS)
rotation was applied to rotate CS of the sample in order to make
them parallel to the view window. Due to photoelectric absorption,
all objects attenuate low-energy X-ray beams stronger than high-
energy X-ray beams. Since beam hardening could lead to
different artifacts in the reconstructed image, beam hardening was
set at 15% in order to reduce artifacts. Reconstructions of the grey
scale histograms were set at a dynamic range of 0.000e0.220 for
potato chip samples. The low grey value within the sample matrix
referred to air cells. The reconstruction time was around 20 min.
2.8.2. Image processing
Segmentation was performed using thresholding, and involved
separating an image into regions corresponding with objects before
morphometrical analysis of the CT images. The technique for seg-
menting a grey scale CT image into a binary image is to define a
global threshold value located at an obvious and deep valley in the
histogram of the grey level frequencies. Voxels with a grey value
lower and higher than that threshold value are considered to be
background and objects, respectively. 3-D image analysis was car-
ried out with CTAn software (V1.15.4.0þ), which computed 3-D
parameters from the stack of 2-D sections after segmentation.
The microstructure of a sample was quantified by utilizing 2-D and
3-D algorithms, resulting in morphometric parameters and geo-
metric 3-D models of the microstructures. The 3-D digital images
(256 grey levels) were analyzed with CTAn, allowing the quanti-
tative characterization of cellular structures. In this study, a 3-D
stack contains 1084 virtual sections, each consisting of
1500  1500 isotropic voxels (¼ 4.83 mm3) with a linear X-ray
attenuation coefficient, and displayed as a grey scale value cali-
brated between 0 and 255 in a histogram. Image processing was
performed by CTAn software. 1084 layers were scanned. The lower
and upper vertical positions were 1.18775 and 7.62534 mm,
respectively. The properties including total VOI volume, object
volume, percent object volume, structure thickness, and number of
closed pores were obtained by the CTAn software.
2.9. Water vapor sorption of potato chips
Water vapor sorption was quantified by the ProUmid SPSx-1m
system (ProUmid GmbH & Co. KG, Ulm, Germany). This instrument
of the SPS series is an integrated system for automatic gravimetric
determination of the water vapor sorption and desorption of
multiple samples in a test atmosphere with controlled temperature
and RH. The adsorption isotherm of samples was measured at
equilibrium at 0e95% RH and 25 ± 0.1
C, and was recorded with a
SPSx-1m moisture sorption analyzer. The time between cycles was
set up as 10 min. The measurement cycle was started at 0% RH and
first increased with a 15% step to 15% RH. Then RH was increased to
30%, 50%, 70%, 85%, and further to 95% RH. The time per cycle was
set to a minimum of 50 min and a maximum of 50 h. If an equi-
librium condition with a constant mass of ±0.01% within 50 min
was reached before the maximum time for all examined samples,
the sequential humidity step was applied before the maximum
time of 50 h. If no equilibrium was achieved, the consecutive hu-
midity step was applied after the maximum time of 50 h. During
the measurement cycle, the samples are automatically placed on an
analytical balance and weighed. The sample pan remains unloaded
and was used for drift compensation of the measured values. The
recorded data were analyzed by SPS-Toolbox Basic Rel. 1.15
120 J. Yang et al. / Journal of Food Engineering 214 (2017) 117e128

software.
2.10. Statistical analysis
The differences in properties including moisture content, oil,
salt and color among different types of potato chips were analyzed
using analysis of variance (ANOVA). The relationship between
moisture content and porosity was evaluated. The moisture content
was considered as response and the porosity as predictor. The RH
was also included into the model as a confounding variable. To have
better confidence in statistical tests, we transformed the left-hand
skewed response using a logarithmic transformation. The porosity
and RH variables were standardized to have comparable scale.
ANOVA lack-of- fit test was performed to validate the model. Each
type of sample was tested at least triplicate. All the analyses used a
significance level 0.05 and were conducted using R.3.2.1.
3. Results and discussion
3.1. Physicochemical properties of three types of potato chips
The physicochemical properties including moisture content, oil,
salt, color, and absolute density in three types of potato chips are
listed in Table 1. There was no difference in moisture content
among the three types of potato chips (p > 0.05). It was observed
that FPC contained the highest oil content, followed by RPC and
BCPC (p < 0.05). There was no statistical difference in salt between
FPC and RPC (p > 0.05). There were no statistical differences
(p > 0.05) in lightness (L value), redness (a value), and yellowness (b
value) between FPC and RPC. However, significant differences
(p < 0.05) in L and a values were found between FPC and BCPC. Less
lightness was monitored in BCPC, due majorly to the intensive
Maillard reaction in this deep frying. No difference in absolute
density was observed among three types of chips (p > 0.05).
3.2. AutoPore mercury intrusion evaluation analysis in potato chips
Porosity is especially important in understanding the formation,
structure, texture, as well as acoustic property of potato chips. The
porosity of a chip affects its physical properties and, subsequently,
its behavior in its surrounding environment. The porosity property
of three types of potato chips is presented in Table 2. Generally, the
total intrusion volume of RPC, FPC, and BCPC were 0.81 ± 0.11,
0.59 ± 0.09, and 0.41 ± 0.08 mL/g, indicating a significant difference
(p < 0.05). Interestingly, there was no significant difference in total
pore area among the three types of potato chips (p > 0.05). RPC
displayed the highest median pore diameter (p < 0.05); while FPC
showed the maximal average pore diameter (p < 0.05). No differ-
ence in apparent density was observed among the three potato
chips (p > 0.05), which was consistent with absolute density. The
results also indicated that RPC exhibited the highest porosity of
50.78 ± 3.02% (p > 0.05), followed by FPC and BCPC.
The relationship between intrusion volumes, pore areas and
pore size diameter in the potato chips is shown in Fig. 1. Specific
cumulative intrusion volume is the absolute volume intruded into
the sample mass divided by the sample mass, therefore normal-
izing the data to each gram of sample. In Fig. 1 (a), it was shown
that, between 300 and 800 mm of pore size diameter, BCPC had the
highest cumulative intrusion volume, followed by FPC and RPC.
Between 70 and 300 mm diameter, FPC exhibited a larger cumula-
tive intrusion volume than that of RPC. Interestingly, below 70 mm,
RPC displayed the highest amount of cumulative intrusion volume
than the other two. The incremental volume VIi for the ith data
point is obtained by finding the difference between two cumulative
values. The two cumulative values define the size boundaries of the
increment. As indicated in Fig. 1 (b), above 400 mm, BCPC had the
highest incremental intrusion volume, followed by FPC and RPC.
Between 250 and 400 mm, FPC was predominant in incremental
intrusion volume. Between 40 and 250 mm, the incremental
intrusion volume in RPC was relatively high. Cumulative specific
pore area is calculated as the sum of the areas determined for each
increment. As shown in Fig. 1 (c), above 90 mm, FPC displayed
slightly higher cumulative pore area with respect to BCPC and RPC,
and showed no significant difference above 200 mm. Under 90 mm,
RPC was observed to have the largest cumulative pore area, fol-
lowed by FPC and BCPC. Differential specific intrusion volume (Vdi)
is calculated by dividing the incremental specific intrusion volume
by the difference in diameters over which the volume increment
was calculated. As shown in Fig. 1 (d), between 15 and 150 mm, the
differential intrusion volume in RPC is dramatically larger than FPC
and BCPC. Using the difference in the logarithms of the size
boundaries, not the absolute difference, normalizes the differential
intrusion data, thus each milliliter of intrusion results in the same
response regardless of the size range. In other words, the net effect
of using the log differential diameter rather than the differential
diameter is that the magnitude of the specific intrusion within the

Table 1
Moisture content, oil, salt, color, and absolute density in the potato chips.

Sample Moisture Content (%) Oil (%) Salt (%) Color Absolute Density (g/cm3)

L a b

FPC 1.72 ± 0.16a 36.26 ± 2.24a 1.71 ± 0.13a 72.17 ± 1.31a 0.61 ± 0.44a 25.28 ± 0.58a 1.2365 ± 0.010a
BCPC 1.57 ± 0.14a 26.14 ± 0.60b 0.90 ± 0.01b 59.88 ± 1.21b 4.11 ± 1.27b 26.59 ± 0.76a 1.2294 ± 0.014a
RPC 1.77 ± 0.05a 31.47 ± 0.74c 1.97 ± 0.06a 71.27 ± 0.81a 0.58 ± 0.64a 26.07 ± 0.50a 1.2566 ± 0.014a

All given values are means of six determinations ± standard deviation (mean ± SD, n ¼ 6).
Means within a column with the same letter are not significantly different (p < 0.05).

Table 2
Porosity property in the potato chips characterized by Mercury Porosimeter.

Sample Total Intrusion Volume Total Pore Area (m2/ Median Pore Diameter (Area) Average Pore Diameter (4V/A) Apparent (skeletal) Density (g/ Porosity (%)
(mL/g) g) (mm) (mm) mL)

FPC 0.59 ± 0.09a 0.04 ± 0.01a 22.84 ± 5.30a 59.72 ± 10.04a 1.20 ± 0.02a 41.15 ± 3.56a
BCPC 0.41 ± 0.08b 0.05 ± 0.01a 9.11 ± 1.82b 33.42 ± 10.01b 1.2 ± 0.03a 32.58 ± 4.21b
RPC 0.81 ± 0.11c 0.06 ± 0.01a 31.46 ± 11.19c 52.84 ± 7.99ab 1.28 ± 0.02a 50.78 ± 3.02c

Values (mean ± SD, n ¼ 6) within a column with the same letter are not significantly different (p < 0.05).
 J. Yang et al. / Journal of Food Engineering 214 (2017) 117e128 121

Fig. 1. The relationship between cumulative intrusion volume (a), incremental intrusion volume (b), cumulative pore area (c), differential intrusion volume (d), Log differential
intrusion volume (e), and pore size diameter (mm) in the potato chips.

increment becomes the dominant factor rather than the diameter
increment. As indicated in Fig. 1 (e), between 600 and 900 mm, the
log differential intrusion volume in BCPC was predominant. There
was a major distribution of log differential intrusion volume be-
tween 400 and 80 mm in FPC. However, the major distribution of log
differential intrusion volume in RPC was between 300 and 20 mm,
showing a fairly normal distribution.
In this study, mercury porosimetry analysis was applied in three
types of potato chips through progressively intruding mercury into
a porous structure under stringently controlled pressures. The
maximal pressure used with the potato chips was around 60 psia
without damaging the structure. The required equilibrated pres-
sure is inversely proportional to the size of the pores. Only slight
pressure is required to intrude mercury into large macropores,
122 J. Yang et al. / Journal of Food Engineering 214 (2017) 117e128

Fig. 1. (continued).
 J. Yang et al. / Journal of Food Engineering 214 (2017) 117e128
whereas much greater pressures are needed to force mercury into
small pores. Even with high pressure, some closed pores with small
sizes may not be penetrated by mercury, resulting in underesti-
mation of total porosity in the three types of chips.
3.3. 3-D analysis of microstructure determined by X-ray mCT in
potato chips
In this study, the distribution of porosity, solids, and oil in three
types of potato chips was characterized by mCT, and is exhibited in
Table 3. RPC had the highest porosity of 66.67 ± 6.06%, followed by
FPC and BCPC, which was in agreement with the data acquired by
Mercury Porosimeter. There was a significant difference in porosity
between RPC and BCPC (p < 0.05); however, no difference in
porosity was observed between RPC and FPC (p > 0.05). Addition-
ally, no significant difference in solids and oil was found among the
three potato chips (p > 0.05). There was no significant difference in
oil content (p > 0.05) quantified by mCT in the three types of potato
chips, which was largely different from results obtained by Soxhlet
extraction. Oil content determined by the wet chemistry method is
more accurate than this imaging method, which could be explained
in that the NMR method detects the elements in chemical structure
of oil to have specificity and uniqueness. The mCT image technique
quantifies oil based on density (histogram), which may include
other components with similar density of oil to overestimate the oil
content.
Fig. 2 displays the distribution of porosity, solids, and oil with
different thicknesses. As shown in Fig. 2 (a), the thickness of
porosity among three potato chips mostly ranged from 0.006 to
1.206 mm. RPC had a large pore diameter, mainly ranging from
0.018 to 0.445 mm. BCPC showed smaller pore diameter, with a
distribution from 0.006 to 1.158 mm. It was revealed that there was
a small to medium size porosity distribution with large thickness
range in FPC. The solids thickness of RPC and FPC had a distribution
range of 0.006e0.255 mm; however, the thickness distribution of
solids in BCPC was from 0.006 to 0.386 mm, as indicated in Fig. 2
Fig. 1. (continued).
123
Table 3
Porosity, solids, and oil distribution in the potato chips characterized by X-ray mCT.
Sample Porosity (%) Solids (%) Oil (%)
FPC 63.13 ± 2.74a 24.87 ± 5.83a 12.00 ± 3.38a
BCPC 54.07 ± 5.60b 34.28 ± 9.49a 11.65 ± 3.91a
RPC 66.67 ± 6.06a 21.55 ± 7.97a 11.77 ± 1.92a
Values (mean ± SD, n ¼ 6) within a column with the same letter are not significantly
different (p < 0.05).
(b). The thickness of oil among the three types of potato chips
mostly ranged from 0.006 to 0.172 mm. RPC showed the largest oil
volume, followed by FPC and BCPC [Fig. 2 (c)]. It was observed that
there was a small amount of oil distributed in the large thickness
range in RPC.
The distribution of cumulative pore, oil, and solids volume with
pore diameter is shown in Fig. 3. The pore diameter of RPC, BCPC,
and FPC was in the range of 100e800, 100e1100, and
100e1300 mm, respectively [Fig. 3 (a)]. Cumulative pore volume
was predominantly 100e500 mm in diameter. BCPC displayed a
large pore diameter range (50e380 mm) of cumulative solid vol-
ume; while both RPC and FPC exhibited a narrow diameter
(50e250 mm) of solids volume [Fig. 3 (b)]. BCPC showed a wide
range of pore diameter (50e460 mm) in cumulative oil volume;
while RPC and FPC had a relatively narrow diameter range of
50e360 mm, and 50e210 mm, respectively [Fig. 3 (c)].
The 2-D and 3-D X-ray micro-tomographic images of three types
of potato chips are shown in Figs. 4 and 5, respectively. When
comparing the images, it is clear that porosity, solids, and oil were
differently distributed in microstructure among the three types of
potato chips. Visually, it was observed that there was more void
space in RPC; while there were more solids in BCPC. In addition, oil
was distributed on the surface of FPC. On the contrary, oil was
internally located in both BCPC and RPC. Porosity is the ratio of pore
volume to apparent volume of the porous medium. Changes in
porosity and the cellular structure of potato chips during
124 J. Yang et al. / Journal of Food Engineering 214 (2017) 117e128

Fig. 2. Porosity (a), solids (b), and oil (c) distributions vs. thickness in the potato chips.

processing are believed to influence processing rates, and thus the
product quality. There exists a strong correlation between porosity
and mechanical properties such as loss modulus and shear strength
for various foods (Gogoi et al., 2000). In our study, BCPC and RPC
had a harder texture; while FPC was crispier. The texture and
mouth feel properties could be ascribed to pore, solid, and oil
distributions.
In this study, higher porosity values were observed in the three
types of potato chips by mCT analysis than by Mercury Porosimeter
(MP) (Tables 2 and 3). These differences are typical when using
different techniques. As previously mentioned, when applying the
MP method, the mercury may not be infiltrated into some closed
pores in the structure. Hence, those pores will be considered as
solids volume, resulting in a lower value for porosity. However, the
mCT method provides data for all types of pores within the 3-D
structure of the material. Therefore, a higher porosity value is ex-
pected when utilizing this method.
Although the porosity data in the three types of potato chips
from X-ray mCT showed trends similar to those measured by the
mercury porosimeter methodology, the absolute values and even
statistical inferences did not match well. This discrepancy is
majorly attributed to the different analytical tools applied: capillary
penetration vs. imaging analysis technique. The former is a well-
established method but limited by the incomplete penetration of
mercury into all pores; while the latter can characterize all pores
but is limited by other components with similar density in the
sample.
As evidenced by the microstructure, RPC contains more pores
 J. Yang et al. / Journal of Food Engineering 214 (2017) 117e128
Fig. 3. Cumulative porosity (a), solid (b), and oil (c) volume vs pore diameter in potato
chips.
125
than FPC and BCPC, which is mainly due to the thickness of the
potato slice and processing conditions. The raw potato slices are
thicker in RPC than in FPC and BCPC, requiring more heat to
evaporate the internal moisture and reach a final moisture of less
than 2% in the finished product. During the above procedure, more
channels in RPC may be generated which drive moisture out,
leading to high porosities.
3.4. Moisture sorption isotherm analysis in potato chips
The shelf life of potato chips depends on the moisture content,
moisture migration, and moisture uptake during storage. Water
vapor sorption change with different RH at 25
C for the three types
of potato chips is presented in Fig. 6. In the climatic chamber of the
system, the samples tested were exposed to different RH values at
25
C. The water uptake was measured by weighing the samples to
find the difference every 30 min. The RH was programed from 0 to
95% in the chamber, which lasted around 165 h. The initial moisture
content of samples was around 1.6e1.8% (Table 1). It was observed
that the change of sample weight in the three types of chips
gradually increased under 70% of RH. Between 70% and 85% of RH,
the three types of chips absorbed water fast, showing a quick in-
crease of water content in a short time. After loading the samples
into the system for about 90 h at 70% of RH, the change in sample
weight of FPC, BCPC, and RPC were 8.01 ± 0.73%, 8.57 ± 0.76%, and
8.59 ± 0.12%, respectively; while the change in sample weight of
corresponding sample increased to 20.29 ± 2.11%, 18.72 ± 1.67%,
and 20.46 ± 1.96%, respectively, at 100 h upon 85% of RH. Between
85% and 95% of RH across from 115 to 165 h, the change in sample
weight of FPC, BCPC, and RPC jumped to 21.25 ± 3.13%,
19.60 ± 1.54%, and 22.48 ± 3.07% to 43.86 ± 8.39%, 38.30 ± 2.65%,
and 46.23 ± 799%, respectively. The water content of three types of
chips reached saturation after storage for 22 h at 95% of RH. It
revealed that water sorption at equilibrium is less or not affected by
the structure.
Equilibrium relative humidity (ERH) is a crucial factor in the
study of the drying process and storage, and is also a valuable tool
in predicting changes in potato chip stability. The extent of sorption
or desorption of water in a product depends on the vapor pressure
of water present in the sample and that of the surroundings. A
previous study showed that water diffusivity of sponge cake was
quite constant near saturation, due majorly to the collapse of the
porous structure (Guillard et al., 2003). A similar trend was dis-
played in our study, suggesting that water transport happened
mainly in the liquid phase within the swollen matrix. However, the
impediment of moisture diffusivity by oil in the potato chips should
be taken into consideration in this study.
The SPS Sorption Test System was designed and developed for
the fully automated determination of the water vapor sorption
isotherm. The water vapor sorption isotherms of the three type
chips at 25
C are shown in Fig. 7. Brunauer et al. (1940) described
five types of isotherms. Type 1 is the Langmuir isotherm. Type 2 is
the sigmoid isotherm observed for soluble products. Type 3 is
known as the Flory-Higgins isotherm, accounting for a solvent or
plasticizer such as glycerol above the glass transition temperature.
Type 4 isotherm describes adsorption by a swellable hydrophilic
solid until the maximum of hydration sites are reached. Type 5 is
the BET multilayer adsorption isotherm. The isotherms most
commonly found in food products are types 2 and 4 (Mathlouthi
and Roge, 2003). Interestingly, in this study it is evident that the
water vapor sorption of the potato chips followed up Flory-Huggins
model (Type 3), which is ascribed to the complexity of matrix in the
126 J. Yang et al. / Journal of Food Engineering 214 (2017) 117e128
Fig. 4. 2-D images identified by X-ray mCT in FPC (a), BCPC (b), and RPC (c) in X-Z, X-Y, and X-Y directions.
Fig. 5. 3-D images identified by X-ray micro CT in FPC (a), BCPC (b), and RPC (c) (white color: salt, green color: solids, orange color: oil, and black color: void). (For interpretation of
the references to colour in this figure legend, the reader is referred to the web version of this article.)
Fig. 6. Moisture content evolution in different RH at 25
C for the three types of potato
chips.
potato chips. This includes semi-crystalline and amorphous areas,
liquid fat, as well as voids, where each of the variables could affect
water migration. It is well known that critical aw plays a pivotal role
in understanding food matrix behavior in shelf life. The results
indicated that the critical aw of the three types of potato chips
ranged from 0.70 to 0.85. At higher aw (above 0.85), RPC displayed
the highest moisture absorption capacity, followed by FPC, and
BCPC. The rate of moisture migration is influenced by the cell size
distribution, interconnectivity of the cells, and the cell wall thick-
nesses (Primo-Martin et al., 2010). The water diffusivity is highly
affected by the volume fraction and the distribution of both solid
and gas phases in porous cereal-based products (Guillard et al.,
2013).
3.5. Relationship between porosity and water vapor sorption in
potato chips
The major external parameters affecting the rate of water
diffusion are temperature associated with the Arrhenius equation,
and RH. On the other hand, the internal parameters modulating
water diffusion are the structure of the potato chips including the
matrix (solid phase), porosity (gas phase), and oil. The relationship
among water content, RH, pore diameter, and total porosity per-
centage, which was determined by Mercury Porosimeter, was
assessed. Fig. 8 shows a higher percentage of porosity was followed
by higher moisture content in the potato chips. We further con-
ducted linear models to investigate the relationship between
porosity and moisture content while the RH level adjusted. Table 4
shows the results after the model selection. The analysis indicated a
significant positive correlation (p < 0.05) between total percentage
of porosity and moisture content of the potato chips. Namely, there
was evidence showing that the higher the total percentage of
porosity, the more water absorbed in the sample. We also observed
significant interaction (p < 0.05) between porosity and RH on
moisture content, where the larger effect of porosity on moisture
content was seen in higher RH. Another linear model using pore
diameter as a predictor showed a significant negative relationship
(p < 0.05) between the square of pore diameter and moisture
content, which indicated that smaller pore diameter was followed
by more water absorption. The previous study conducted by
Guillard et al. (2003) indicated that the smaller the size of the pores
in the matrix of the food domain, the slower the moisture
migration.
Porosity in particular influences the water diffusion rate. If
porosity is predominant in the food matrix, water molecules
transfer quickly due to capillary action and vapor diffusion in the
pores. On the other hand, in a low-porosity food, liquid diffusion is
the principal way of moisture migration. Experimental data
 J. Yang et al. / Journal of Food Engineering 214 (2017) 117e128 127

Fig. 7. Water sorption isotherm at 25
C in the potato chips.

suggested that moisture and oil migration in porous food matrices

is driven by the capillary pressure governed by the Laplace-Young
equation (Carbonell et al., 2004). The relationship among water
content, RH, oil, and porosity percentage determined by mCT was
evaluated. The X-ray mCT system showed results consistent with the
Mercury Porosimeter (Fig. 8). Here, we included both RH and oil
content into the model (Table 4). The statistical analysis showed
that the increase in total percentage of porosity was followed by the
increase in moisture content of potato chips among the same RH
and oil level. We also observed that the oil content significantly
blocked water sorption in the sample (p < 0.05). The significant
interaction (p < 0.05) between porosity and RH on moisture content
was also monitored, indicating there was a larger effect of porosity
on moisture content in higher RH. Reducing food porosity tends to
slow down water diffusion. For example, decreasing the porosity of
the cereal compartment in a composite food significantly lowered
the internal moisture diffusivity by at least a factor 2 (Roca et al.,
2007). Generally, these findings could provide some guidance in
improving product design, process optimization, texture, and shelf
life of fried potato chips.

4. Conclusion

Fig. 8. Box plot of moisture content among different total porosity percentage quan-
tified by both Mercury Porosimeter and X-ray mCT methods.
The microstructure of a potato chip affects its physical proper-
ties and, subsequently, its behavior in its surrounding environment.
The results indicated that RPC showed the highest porosity,

Table 4
Relationship between porosity and moisture content measured using both Mercury Porosimeter and X-ray mCT methods.

Mercury Porosimeter X-ray mCT

Porosity Percentage Pore Diameter Porosity Percentage

Coefficient p-value Coefficient p-value Coefficient p-value

Porosity Percentage 0.044 0.003 e e 0.071 <0.001

Porosity diameter e e 0.003 0.097 e e
Porosity diameter2 e e 0.097 0.002 e e
Relative humidity 1.054 <0.001 1.054 <0.001 1.054 <0.001
Relative humidity2 0.192 <0.001 0.192 <0.001 0.192 <0.001
Relative humidity3 0.156 <0.001 0.156 <0.001 0.156 <0.001
Interaction 0.031 0.038 0.027 0.065 0.032 0.031
Oil e e e e 0.049 0.022
Intercept 1.577 <0.001 1.827 <0.001 1.577 <0.001
128 J. Yang et al. / Journal of Food Engineering 214 (2017) 117e128
followed by FPC and BCPC. The solids distribution in RPC, FPC, and
BCPC were 21.56 ± 7.97%, 24.87 ± 5.83%, and 34.28 ± 9.49%,
respectively. mCT cross-section images displayed a highly porous
microstructure in FPC, while RPC appeared to have thicker walls
and larger cells than the others. RPC also exhibited a higher pres-
ence of large pores than those in the other two potato chips.
Accurately determining water sorption isotherms is critical for
appropriate development and storage of potato chips. The data
suggested that the critical aw of the three types of potato chips
ranged from 0.70 to 0.85. The porous structure of potato chips has
an important effect on quality and moisture migration. The results
revealed that a higher percentage of porosity is followed by higher
moisture content in potato chips. A larger effect of porosity on
moisture content was monitored in higher RH. The oil content
significantly blocked water sorption in the sample (p < 0.05). It
proposes that water vapor sorption of the potato chips was gov-
erned by the Flory-Huggins model. These findings help to under-
stand the frying mechanisms, improve the quality, and extend shelf
life of fried potato chips.
Conflicts of interest
The authors declare no conflict of interest.
Acknowledgements
The authors thank Dr. Pawan Takhar for technical comments and
suggestions.
References
Alam, T., Takhar, P.S., 2016. Microstructural characterization of fried potato disks
using X-ray micro computed tomography. J. Food Sci. 81 (Nr. 3), E651eE664.
Alvarez, M.D., Canet, W., Tortosa, M.E., 2001. Kinetics of thermal softening of potato
tissue (cv. Monalisa) by water heating. Eur. Food Res. Technol. 212, 588e596.
Baik, O.-D., Marcotte, M., 2003. Modeling the moisture diffusivity in a baking cake.
J. Food Eng. 56, 27e36.
Basu, S., Shivhare, U.S., Mujumdar, A.S., 2006. Models for sorption isotherms for
foods: a review. Dry. Technol. 24, 917e930.
Brunauer, S., Deming, L.S., Teller, E., 1940. On a theory of Van der Waals adsorption
of gases. J. Am. Chem. Soc. 62, 1723e1732.
Carbonell, S., Hey, M.J., Mitchell, J.R., Roberts, C.J., Hipkiss, J., Vercauteren, J., 2004.
Capillary flow and rheology measurements on chocolate crumb/sunflower oil
mixtures. J. Food Sci. 69, E465eE470.
Costa, R.M., Oliveira, F.A.R., Boutcheva, G., 2001. Structural changes and shrinkage of
potato during frying. Int. J. Food Sci. Technol. 36, 11e23.
Dogan, H., Kokini, J.L., 2007. Psychophysical markers for crispness and influence of
phase behavior and structure. J. Texture Stud. 38, 324e354.
Gogoi, B.K., Alavi, S.H., Rizvi, S.S.H., 2000. Mechanical properties of protein-
stabilized starch-based supercritical fluid extrudates. Int. J. Food Prop. 3, 37e58.
Gueven, A., Hicsasmaz, Z., 2013. Pore Structure in Food: Simulation, Measurement
and Applications. Springer Publisher.
Guillard, V., Bourlieu, C., Gontard, N., 2013. Food Structure and Moisture Transfer: a
Modeling Approach. Springer Publisher.
Guillard, V., Broyart, B., Bonazzi, C., Guilbert, S., Gontard, N., 2003. Moisture diffu-
sivity in sponge cake as related to porous structure evaluation and moisture
content. J. Food Sci. 68, 555e562.
Herremans, E., Verboven, P., Bongaers, E., Estrade, P., Verlinden, B.E., Wevers, M.,
et al., 2013. Characterisation of ‘Braeburn’ browning disorder by means of X-ray
micro-CT. Postharvest Biol. Technol. 75, 114e124.
Ho, Q.T., Verboven, P., Fanta, S.W., Abera, M.K., Retta, M.A., Herremans, E.,
Defraeye, T., Nicolaï, B.M., 2014. A multiphase pore scale networkmodel of gas
exchange in apple fruit. Food Bioprocess Technol. 7, 482e495.
Lape, A., Jensen, S., Jeor, V.S., Lendon, C., 2008. Use of X-ray micro computed to-
mography in the evaluation of bread crumb structure. Microsc. Microanal. 14,
700e701.
onard, A., Blacher, S., Nimmol, C., Devahastin, S., 2008. Effect of far-infrared
Le
assisted drying on microstructure of banana slices: an illustrative use of X-ray
microtomography in microstructural evaluation of a food product. J. Food Eng.
85, 154e162.
Mathlouthi, M., Roge, B., 2003. Water vapour sorption isotherms and the caking of
food powders. Food Chem. 82, 61e71.
Ormerod, A., Ralfs, J., Jobling, S., Gidley, M., 2002. The influence of starch swelling on
the material properties of cooked potatoes. J. Mater. Sci. 37, 1667e1673.
Primo-Martin, C., van Dalen, G., Meinders, M.B.J., Don, A., Hamer, R.H., van Vliet, T.,
2010. Bread crispness and morphology can be controlled by proving conditions.
Food Res. Int. 43, 207e217.
Rao, K.J., Dhas, P.H.A., Emerald, F.M.E., Ghosh, B.C., Balasubramanyam, B.V.,
Kulkarni, S., 2006. Moisture sorption characteristics of chhana podo at 5
C and
35
C. J. Food Eng. 76, 453e459.
Rizzolo, A., Vanoli, M., Cortellino, G., Spinelli, L., Contini, D., et al., 2014. Charac-
terizing the tissue of apple air-dried and osmo-air-dried rings by X-CT and OCT
and relationship with ring crispness and fruit maturity at harvest measured by
TRS. Innov. Food Sci. Emerg. Technol. 24, 121e130.
Roca, E., Broyart, B., Guillard, V., Guilbert, S., Gontard, N., 2007. Controlling moisture
transport in a cereal porous product by modification of structural or formula-
tion parameters. Food Res. Int. 40, 461e469.
Roca, E., Guillard, V., Guilbert, S., Gontard, N., 2006. Moisture migration in a cereal
composite food at high water activity: effects of initial porosity and fat content.
J. Cereal Sci. 43, 144e151.
Takhar, P.S., & Zhang, S. (2009). Drying of corn kernels: from experimental images
to multiscale multiphysics modeling. Comsol Conference Proceeding.
van Dalen, G., Koster, M., Nijsse, J., Boller, E., & van Duynhoven, J. (2013). 3D imaging
of freeze-dried vegetables using x-ray microtomography. Proceedings of the
Micro-CT user meeting SkyScan. Belgium: Hasselt.
van Dalen, G., Nootenboom, P., van Vliet, L.J., Voortman, L., Esveld, E., 2007. 3D
imaging, analysis and modelling of porous cereal products using X-ray micro-
tomography. Image Anal. Stereol. 26, 169e177.
Zhu, L.-J., Dogan, H., Gajula, H., Gu, M.-H., Liu, Q.-Q., Shi, Y.-C., 2012. Study of kernel
structure of high-amylose and wild-type rice by X-ray microtomography and
SEM. J. Cereal Sci. 55, 1e5.