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Achieving food products performance by mastering the drying process

Conference Paper · August 2014

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ACHIEVING FOOD PRODUCTS PERFORMANCE BY MASTERING THE DRYING
PROCESS

A. Gianfrancesco1*, T. Kockel1, S. Palzer2

1
Nestec Product Technology Centre Konolfingen
Nestlé Strasse 3, 3510 Konolfingen, Switzerland
2
Nestlé Beverages Business Unit, Av. Nestlé 55, 1800 Vevey, Switzerland

*Corresponding author: Tel.:+41 31 790 1147, E-mail: [Link]@[Link]

Abstract: A wide majority of food products requires a drying step at one moment of their
production. There is therefore a strong interest of the food industry in continuously
improving the understanding of the drying process in order to guarantee high quality
products together with manufacturing excellence.
Apart from its obvious function of removing water, drying can be seen as a structuring
process in which specific attributes are generated. For instance, defined texture, color or
flavors can be achieved by the appropriate choice of the drying technology and the
process parameters. Considering food powders, their flowing and reconstitution behavior
is strongly dependent on the physical structure and surface attributes which are created
along drying.
A good understanding of the link existing between material properties and process
parameters will also help preventing loss of viable nutrients during drying and ensuring
stability during subsequent storage and shelf-life.
In this work we aim at reviewing several examples of how it is possible to improve the
quality of food products by establishing links between process, material properties and
final performance. We will discuss examples covering optimization of product’s
appearance, sensorial perception and nutritional value.

Keywords: drying, food, structure, performance, throughput

INTRODUCTION
Understanding and controlling the drying process is
of particular relevance for the food industry, as most
For instance, a complete and fast dissolution is
of its products undergo a drying step during their
expected from soluble powders, either in hot or cold
manufacturing. These include – among many others
liquid. For other applications, a defined appearance
– soluble food powders (like coffee, milk and dairy
specialties, cocoa, or soups), ingredients (spices, (color, shape) could be required for better appealing
herbs, proteins, lactose etc.) or solid products (e.g. products.
pasta, wafers, and confectionary products). During processing, specific flavor and aroma profiles
can also be generated; controlling the drying
A huge choice of dryers is commercially available,
parameters is therefore important to avoid unwanted
varying from simple evaporators to spray dryers,
product’s degradation or – on the other hand – to
roller dryers, freeze dryers, vacuum belt dryers and
several others. So the question of choosing the right reach the desired sensory profile.
process for every specific application arises. Apart
In the past decade, considerations linked to nutrition,
from its obvious function of removing the excess of
health and wellness have become increasingly
water present in the product according to its
important for the food industry. For this reason an
manufacturing specifications, drying must be also
additional requirement associated to successful
considered as a structuring process.
drying, is to preserve and improve the nutritional
For this reason, the choice of the right dryer depends quality of the final products. For instance,
strongly on the possibility of obtaining the desired degradation of sensitive components like vitamins or
final performance. probiotic strains should be avoided or minimized by
carefully choosing the right processing conditions.
Due to health regulations and consumer perception, temperature Tg) and hygrostability (link between Tg
food industry is actively engaged in reducing sugar and water activity). On the other hand, crystalline
and salt content in its products. However, perceived materials like sucrose are less sensitive to humidity
sweetness or saltiness is often a key parameter to and do not exhibit a glass transition. Drying
obtain consumer preference. For this reason, it is not conditions could be used to create specific physical
sufficient to simply reduce the amount of sugar and states.
salt in actual recipes, as the resulting sensory profile
Improving dissolution of sucrose coatings
could be unacceptable. Thus an important effort in
research and development is actually put in the
If we consider sucrose, its stable form is the
development of more healthy products without
crystalline one due to its very low glass transition
compromising on sensory attributes. The correct
temperature[1].
handling of the drying process is part of this
However, it is known that crystalline materials have
development. Any recipe’s modification can in fact
often longer dissolution times compared to
lead to technical problems such as density changes
amorphous[2], so that it would be interesting to
(with influence on packaging), different flowing or
produce a stable amorphous sucrose which would
reconstitution problems.
dissolve faster both in liquids (e.g. milk, water) and
in mouth. A faster dissolution could also potentially
In order to reach all the cited objectives, it is
lead to an enhanced sweetness perception.
necessary to gain a full understanding of the
evolution of product’s properties all along the drying.
The main technical challenge is linked to the
This includes characterizing the material to be dried
production of such an amorphous sugar by avoiding
in terms of composition and specific material
crystallization during the process. Vuataz[3] showed
properties such as moisture content, water activity,
how state diagrams can be used to represent the spray
glass transition, fat melting profile etc. These
drying pathway of milk and avoid lactose
properties should then be linked to the specific
crystallization. It is necessary to cross very fast the
drying kinetics and other process characteristics
region in between the solubility line and the glass
depending on the chosen drying technology.
transition, in which crystallization could occur in few
Modelling can also be an important tool to help
minutes. Once below glass transition, the product
product developers in the choice of the right
will remain in the amorphous state without
processing parameters.
crystallizing if its temperature remains below Tg.
It is also possible to aim partial crystallization in a
The final goal for a successful industrial development
fluid bed dryer after spay drying, to improve for
should be to conciliate the already cited quality
instance the flowing behavior of the final powder.
attributes without compromising on the dryer’s
This fast drying is usually obtained by spray drying,
throughput and energetic efficiency. In this review
as in the case of milk. However, spray drying is not
we will analyze some examples showing how the
suitable to dry small sugars as pure sucrose without
understanding of material properties could be linked
drying aids (e.g. high molecular weight
to the analysis of the drying process in order to
carbohydrates), due to their very low glass transition
achieve this challenging objective.
temperature leading to a pronounced sticky behavior.
For this purpose, freeze drying could be a more
ACHIEVING FUNCTIONNALITY BY DRYING
suitable process, as discussed in Gianfrancesco et al.
[4]
During drying, the product can undergo several . The freeze drying experiments performed on
chemical and physical transformations – such as sucrose-coated model materials led to different
Maillard reactions or crystallization – which will drying paths which could be represented on a state
have an important impact on the final performance diagram of sucrose (Fig.1). Due to the experimental
attributes. It is possible to modulate the drying set-up limitations, measurements of the drying
process in order to produce or to avoid specific kinetics were possible only when the temperature
reactions. In this section we are showing how to was higher than -40°C.
control sucrose crystallization to enhance solubility
and how to avoid unwanted degradation reactions to
preserve the nutritional value of a food powder.
It is at first necessary to make a distinction between
amorphous and crystalline structures, which will
exhibit very different behaviors especially in terms of
dissolution and stability. Amorphous materials
constitute a wide majority of the commercially
available food powders. Their behavior is strongly
influenced by their hygrocapacity (sorption
isotherms), hygrosensitivity (glass transition
 State Diagram of sucrose (2006) trial III (slowest drying) had a spectrum similar to the
30
25
amorphous reference, while the samples dried faster
20
15 exhibited a crystallization peak.
10
5 Trial I
0 0.60
-5 Reference and FD samples
1 Pa.s Sucrose
Temperature [°C]

-10 Trial III 2014.025 cyst.

-15 cr
-20 Tg
015-powder
-25 Tfp 0.59 - FD trial 1
1 KPa.s
-30
Tsol
- FDSCtrial 2
- FD - 4°C/h
1000
-35 1 MPa.s
10000
- FDLCtrial 3 Freeze drying rate

Normalized absorbances
- FD 1.25°C/h
-40 100000 - Amorphous ref.
-45 1000000 0.58 - Crystalline
Crystalline ref. ref.
-50 10000000
100000000
-55
1000000000
-60
10000000000
-65
Tg 1E+11
0.57
-70 Tg line 1.25 °C/h

-75 4°C/h
am
-80
70 75 80 85 90 95 100

Concentration [%] 0.56

Fig. 1. State diagram of sucrose with measured freeze

drying kinetics. 0.55
1400 1410 1420 1430 1440 1450 1460 1470 1480
Raw data f rom MPA

1490 1500
Wavelength [nm]

It can be seen that during the faster drying kinetics

(trial I), the product temperature remains above the Fig. 3. NIR spectra of freeze-dried samples
glass transition line during most of the process, so
that some crystallization could be possible in these These differences can be seen in the microscope
conditions. The slowest drying path (trial III) allowed images of the samples (Fig.4). Sucrose crystals
maintaining the sucrose below Tg for a longer time. appear in bright under polarized light, so that the
bigger amount of crystallization due to faster drying
The different samples were compared to a crystalline can be observed.
and an amorphous reference, to qualitatively assess
their crystallization degree. In a DSC thermogram
(Fig.2), the presence of amorphous sucrose leads to
the observation of an endothermic glass transition
followed by an exothermic crystallization peak, while
this peak is not observed if all the sucrose is already
crystalline. The importance of the peak could also
give an idea of the relative amount of still amorphous
sucrose present in the different samples. For instance,
it can be observed that the samples freeze dried in the Fig. 4. Pictures of freeze dried samples under
slower conditions (trial III) showed a bigger polarized light; sucrose’s crystals appear in bright.
crystallization peak, indicating the presence of a (left): trial I; (right): trial III.
higher amount of amorphous sucrose.
This qualitative result was confirmed by NIR As a conclusion, it was possible to produce a mostly
measurements and microscopy observations under amorphous sucrose coating by applying slow freeze
polarized light. drying kinetics. However, crystallization could never
be completely avoided. Part of the sucrose could
-0.01
Sucrose-coated cereals - freeze dryed
already crystallize before drying, during the coating
-0.02 Exothermic process although this was very fast (2 minutes).
crystallization peaks
-0.03
Spray coated - FD - 22/1/2010 Some crystallization could then occur during freeze-
Liquid coated - FD - 12/2/2010

-0.04
Crystalline reference drying, depending on the product temperature during
primary (sublimation) and secondary (desorption)
Heat flow [W/g]

-0.05

-0.06
drying. As the maximum cryoconcentration of
-0.07 Trial I sucrose is 83%, this means that in the discussed
-0.08
experiments 10% of the initial water content would
Trial III
-0.09
be in ice form and sublimate, while 17% of water
-0.10
Glass transition would remain unfrozen and should be removed by
-0.11
desorption in the second period of drying.
25 30 35 40 45 50 55 60
Temperature [°C]
65 70 75 80 85 90 95
During sublimation, the product temperature is
mostly dependent on the chamber pressure; for pure
Fig. 2. DSC thermograms of freeze dried samples. water, the sublimation temperature imposed by a
pressure of 13 Pa is close to -40°C, which is higher
NIR spectrum showed a peak linked to the presence than the sucrose’s glass transition at its maximal
of crystalline sucrose at a wavelength of 1440 nm cryoconcentration. Thus part of the sucrose could
(Fig.3). A clear trend in the relative amount of crystallize, although the high viscosity and the small
amorphous sucrose as a function of the freeze drying amount of water to sublimate suggest than
rate could be observed. Samples produced during
crystallization during primary drying should be
neglectable.
Thus, the main responsible for crystallization seems
to be the secondary drying, if the product’s
temperature exceeds Tg. Monitoring the drying
kinetics and applying a smooth temperature increase
allows to guarantee the equilibrium between product
and plate temperature and to follow the Tg line in
order to mostly avoid crystallization.

The stability of the coating at ambient temperature

and relative humidity was checked after 3 weeks, and
the amorphous state could be maintained with the
adequate packaging and storage conditions. Faster
sugar dissolution in liquid compared to the crystalline Fig. 5. Heat-induced lysine loss at a water activity of
reference could be put into evidence. 0.43 at 25°C, i.e., a water content of 8.54 ±0.07% wb

Preservation of nutritional value along drying As it could be expected, lysine losses increased with
increasing heating temperature and at prolonged
For many food products, preservation of nutritional heating times, with a sharp increase in the first 2-3
value during the processing is a key requirement. The minutes. However, the temperature dependence as
drying step could potentially harm the products, if well as the extent of lysine loss depended on the
they contain sensitive ingredients which could be concentration and on the physical state of the system.
damaged by exposure to high temperature, oxygen or
dehydration rates. For instance, spray drying is one Fig. 6 shows the extent of lysine loss after 30 min of
critical production step concerning lysine loss during heating, for different water activities (i.e. water
the production of infant formulae. Lysine is an content). It can be observed that a different maximum
essential amino acid and as such it is often the in lysine losses can be distinguished for each
limiting factor regarding the nutritional value of temperature, except at 60 °C where there was no
food. However, it can only be metabolized by the significant impact of the water activity. At 70 °C the
human body if its ε-amino group is free. The main maximum is found at a water activity of about 0.43.
cause for lysine degradation is the early Maillard- At 80 °C and 90 °C, the maximum is shifted to lower
reaction between a reducing sugar, e.g. lactose in water activities in the range of 0.2. These differences
milk products, and the amino group of lysine which are due to the physical state of the system, which is
leads to the formation of the Amadori product. Infant mainly linked to the state of the lactose.
formulae contain lysine-rich proteins but also high
amounts of lactose, so that preventing lysine loss is
essential for this product’s category.
[6]
The work of Schmitz et al. focused on the
understanding of the lysine degradation during
drying of model dairy formulations, by distinguishing
between losses due to exposure too high temperatures
and the ones associated to the dehydration rate.
During spray drying particle experiences a series of
temperature-concentration-time-combinations which
will lead to a certain extent of lysine loss depending
on their material properties. Lysine loss kinetics were
thus established and linked to the physical state of the
formulation, i.e. mainly the physical state of lactose.

Fig. 5 shows the impact of temperature on lysine Fig. 6. Lysine loss after 30 min of heating as a
[6]
losses at a fixed concentration. In the original study function of the concentration and the physical state
freeze-dried samples were equilibrated at different
water activities (0.06 to 0.75) and then heated in Lactose is a small molecule which undergoes glass
closed sample holders to 60 – 90 °C for 0.5 – 30 min. transition and can therefore be in the glassy or
crystalline state depending on the experimental
conditions. When heated above its Tg for sufficient
long time, the molecule will be in a unstable rubbery
state which will eventually lead to crystallization. In
this condition, the molecular mobility is maximal,
and the chemical reactivity is also enhanced. This step is called primary drying. But part of the
Therefore the maximum of lysine losses was water is not frozen and remains bound to the cryo-
observed in this transition region. On the other hand, concentrated solid matrix. This water should be
once the lactose is in the crystalline form its evaporated by desorption during the so-called
availability for the early Maillard reaction with the secondary drying. It should be noted that these steps
amino group of lysine is again reduced and lower are not sequential, and could indeed occur in parallel
losses are measured. to some extent[7].
From the above results, it can be concluded that to The sublimation of the ice crystals leads to a final
preserve the available lysine the spray drying porous structure, which is usually easy to rehydrate.
parameters should be optimized in order to avoid The final porosity can also be increased by adding a
long residence time of powders with a temperature gassing step before drying (e.g. for soluble coffee). In
above glass transition. In fact, in industrial spray order to maintain the desired porosity, density and
dryers some particles could have residence times of visual appearance of the final product, it is important
up to 30 minutes, especially the recirculated fine to guarantee that the product's temperature is
particles. These particles will have a temperature maintained below a critical collapse temperature Tc'
close to the exit air temperature, which is typically in along the whole process. This value is normally
the range of 70 to 90°C. According to the physical linked to the glass transition temperature of the
state diagrams and the above considerations, it is cryoconcentrated matrix Tg', and can be measured by
therefore important to carefully choose the exit air differential scanning calorimetry or by direct
temperature in order to avoid being in the peak observation with cryomicroscope[8]. For many food
region for the lysine losses kinetics. It is also possible materials, Tc' is in the range between -20 and -
to optimize the atomization parameters and the 30°C[5,8].
agglomeration degree inside the tower by adjusting
Due to the high energetic cost of freeze drying, the
process parameters and configuration (e.g. nozzle
optimization of the drying time while avoiding
position). In this way the creation of fine particle and
product degradation is essential for industrial
their recirculation with long residence time could be
applications, especially in the food industry[8]. While
minimized.
the product's temperature should remain below Tc
during primary drying, once the sublimation is
completed it is possible to increase the amount of
ACHIEVING HIGHER THROUGHPUT
heat provided to the product in order to accelerate
In the previous section we have reviewed some desorption of the bound water[9]. But the temperature
examples about how it is possible to generate specific increase should be modulated as a function of the
functionalities by adapting the drying profile. specific material properties like glass transition, in
However, for industrialization purposes it is equally order to avoid collapse of the matrix[10].
important to maximize the throughput of the drying
As already shown in the previous section, the
process. Again, the understanding of material
characteristic drying behavior of a specific material
properties is paramount to reduce drying times while
can be measured by following its weight evolution
maintaining an optimal product’s quality. In this
along drying. The recorded drying kinetics can then
section we are discussing two additional examples
be represented on a state diagram[9], to determine
concerning optimization of freeze drying and spray
possible optimization of the drying parameters,
drying processes.
especially after the completion of ice sublimation. An
Optimization of freeze drying cycles ideal freeze drying cycle will consist in maintaining
the sample temperature just below its Tc’ along the
Since the advent of industrial freeze drying, this sublimation phase, followed by a regular increase in
technique has been associated with superior product's
the sample temperature following the Tg line when
quality and to preservation of freshness and active
the concentration is higher than Cg’(i.e sublimation
principles. This is in particular linked to the fact that
is completed). In this way, it was for instance
water can be removed while maintaining the product
possible to reduce by half the drying time of a model
at low temperature along the whole process. This soluble powder [4].
process is widely used by the pharmaceutical
industry for production of different medicaments, as Measurements of drying kinetics are helpful for
well as by the food industry for drying of vegetables, determining the switch between primary and
fruits and soluble coffee among others applications. secondary drying, but they do not provide any
information about the freezing step, during which the
During a classic freeze drying cycle, the product to
sample's weight remains constant. However, freezing
be dried is first frozen at ambient pressure, so that a plays an essential role as the size of the ice crystals
majority of the water content (~70-80%) freezes in produced determine the subsequent drying rate [5,7].
order to form ice crystals. After this first step, the
pressure is decreased and heat is provided to the Moreover, the freezing of the material is associated
samples so that the frozen water could sublimate. to a concentration of the solid matrix, which can be
detrimental to the final structure and properties. In Avoid stickiness during spray drying
pharmaceutical applications, several excipients are
In spray drying operations, one major limitation
often used as cryoprotectants[5,10]. But in food
which needs to be taken into account is the possible
applications, modification of the original recipe is
fouling of the tower (Fig. 8). When not correctly
often not possible and an accurate control of the
prevented, this can provoke complete blockage of the
freezing conditions (time, temperature, velocity) is
tower with considerable negative economic
even more necessary.
consequences. Fouling is caused by powder sticking
In order to assess the influence of the freezing to the walls of the dryer, especially in the cone or in
conditions on the drying behavior, thermal analysis the cyclone. Thus, understanding and controlling the
could be a useful technique. By coupling development of stickiness is essential in order to
themogravimetry with differential scanning choose the right spray drying processing parameters.
calorimetry (TG-DSC), it is possible to measure at
the same time the weight evolution (i.e. drying
kinetics) as well as the thermal signal associated to
the formation of ice crystals and the sublimation and
desorption of water[11,12].

By applying this technique it was for instance

possible to put into evidence a different freezing
behaviour of two different maltodextrin solutions
(DE 6 and DE 40) exposed to the same temperature
profile (Fig. 7).
Fig. 8. Powder stickiness observed on the wall of an
30 100
industrial spray dryer.

20
Spray dryers are usually operated by controlling the
80
inlet and outlet temperature (Tin and Tout), and
10
Température (°C)
adjusting the others parameters (e.g. liquid flow rate,
60
Température (°C)
air flow rate, air temperature) accordingly to the set
Temperature (°C)

Heat flow (mW)

Heat flow MD 40 (mW)

0 Heat flow MD 6 (mW)

40
point value. The choice of this value depends
-10 primarily on the amount of water that needs to be
20 removed (according to the water mass balance), but it
-20
is also influenced by the sticky behavior of the
-30
0 considered material. It can be assumed that the
powder in the drier will equilibrate with the
-40 -20
0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 surrounding air, so that its surface temperature and
Time (min)
water activities will be equal to the exit air
Fig. 7. Thermal signal recorded during freezing of temperature and relative humidity. It is thus
aqueous maltodextrin DE6 and DE40 solutions. important to characterize the adhesion behavior of
the dried substance in the relevant range of
Comparing the thermal signals along freezing, it can temperature and moisture content.
be seen that maltodextrin DE 6 exhibits two different
peaks of crystallization. This suggests the presence of The measurement of glass transition is normally used
two subsequent nucleation steps, thus leading to a as key parameter to predict possible stickiness during
higher amount of small ice crystals in comparison drying (and storage). It is commonly assumed that a
with MD DE 40. As a consequence, the initial drying powder will stick when its temperature is about 20°C
rate of maltodextrin DE 6 solutions during primary higher than Tg. However, the glass transition concept
dryer was higher due to the bigger specific surface of is valid only for pure carbohydrate. The presence of
ice. other components like proteins and fats can lead to
different sticky mechanisms. Furthermore, stickiness
Thus the analysis of the thermal signal can provide is a surface property, while Tg is measured on the
an additional insight about what happens to the whole powder. So for instance two powders with the
solution during freezing, which is not possible in same carbohydrate profile and the same average
batch freeze drying experiments. As a consequence, moisture content will exhibit the same Tg, even if in
different freezing conditions (T, time) can be tested practice their sticky behavior could be strongly
in order to identify the better ice structure to different. Gaiani et al. have measured how the
accelerate water sublimation during primary drying. surface composition of powders could significantly
differ from the bulk composition, depending on the
applied drying conditions[13]. It is this surface
composition which is important in determining the is still a challenge and opens new perspectives for the
sticky behavior along the process. further development of the science of drying.
While several methods to measure powder stickiness
ACKNOWLEDGMENTS
are reported in literature [14], it should be noticed that
as “stickiness” is not a defined physical property, the
I would like to thank Dr. Iris Schmitz, Katarina
choice of the right method depends on the specific
Slettengren and Jean-Christophe Andrieux who
application considered. For spray drying purpose, a
performed several of the experiments described or
suitable choice can be the use of an adapted powder
rheometer, in which the temperature of the sample is cited in this paper.
progressively increased until that a sharp increase in
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