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International Journal of Food Science and Technology 1999, 34, 335342

Wetting behaviour of instantized cocoa beverage


powders
P. Kyaw Hla1 & S. Hogekamp2*
1 Department of Industrial Chemistry, University of Yangon, University P.O., Yangon, Myanmar, Southeast Asia
2 Institut fr Lebensmittelverfahrenstechnik, Universitt Karlsruhe, Kaiserstr. 12, D-76131 Karlsruhe, Germany

(Received 7 December 1998; Accepted in revised form 2 April 1999)

Summary

The aim of this work was the characterization of various instantized cocoa beverage powders with regard to their wetting behaviour in a standardized test. Brand name powders
from local superstores were compared to each other and to model powders instantized in
the laboratory by steam jet agglomeration. Basic powder properties such as agglomerate
size or fines content in a mixture were varied to study possible effects on the wettability
of this product group.

Keywords

Steam jet agglomeration, wetting time.

Introduction

Agglomeration is one of the instantization


processes most frequently used. Agglomeration
also may improve the handling properties and the
appearance of the powder. Instantized or
instant means that agglomerated beverage powders (e.g. instant coffee, dry milk, cocoa-based
beverages) are supposed to be dispersed or dissolve quickly in water or in milk (Schubert, 1993),
i.e. after stirring the product in the liquid for a
short time, the particles neither float to the surface nor sediment to the bottom of the container
within a certain time and no excessively large particles are left.
For a beverage powder with good instant properties, wetting, sinking, dispersing and dissolving
of a powder layer are completed within a few seconds for a layer height of, for example, 10 mm.
The wetting time can be shortened primarily by
increasing the particle size by agglomeration.
Agglomerate structure is also important, as the
liquid must also wet the agglomerate itself to

*Correspondent: Fax: +49 721 694320;


email: stefan.hogekamp@ciw.uni-karlsruhe.de

1999 Blackwell Science Ltd

achieve a good dispersibility. The agglomerate


size should therefore not exceed a certain range
(12 mm). If the agglomerates are smaller than
the optimum size, the material is wetted too slowly (Schubert, 1993).
Not all agglomeration processes are suitable for
the attainment of good instant properties. In
instant food production process, the following
types of agglomeration occur: agglomeration of
wetted single particles, agglomeration by drying,
combination of both of these methods, and
agglomeration by compression (Schubert, 1979).
Agglomeration by wetting is mostly used for
making instant food products. The main processes used for making instant products in agglomeration by wetting are fluidized-bed, agitation, or
steam jet agglomeration and related methods.
The most favourable process for treating food
products is steam jet agglomeration, which uses
condensing steam for wetting the powder. Only a
very short residence time is required, so that
flavours have less time to escape. Steam jet
agglomeration, however, is only successful if
practically every interparticle collision also leads
to adhesion. Otherwise no agglomerates of sufficient size can be formed. Also, pre-agglomerates
should already be present in the feed. These are

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Wetting behaviour of instantized cocoa P. Kyaw Hla & S. Hogekamp

then stabilised by the steam treatment.


Agglomerates formed by this process have a high
porosity and good wettability but also an acceptable strength for handling and packaging
[Hogekamp, 1997, pp. 148152].
Among the instantized beverage powders available in Europe, cocoa beverage powders play an
important role. The products available on the
German market consist essentially of sucrose, glucose (may be replaced by sucrose in other
European countries), low-fat cocoa and several
minor ingredients. The total proportion of sugars
in most products is about 80%. Due to the high
sugar content, good instant properties are possible. In order to be able to attain good wettability, cocoa with strongly reduced fat content
(, 15%) is used. Lecithin (0.52%) is added to
further improve wettability and dispersibility (a
method also frequently applied to improve the
properties of whole-milk powder). The results
vary widely due to different recipes (the type of
cocoa e.g., having a strong influence) and manufacturing methods (milling, lecithination, agglomeration process).
In the present work, a more detailed investigation into the wetting behaviour of agglomerated
cocoa beverage powders under different circumstances is made. The objectives of the experiments

were to show basic effects influencing the quality


of instantized cocoa beverage powders, to get an
impression of the quality range of currently available instant powders, and to compare brandname products to powders produced in the
laboratory using steam jet agglomeration.
Materials and methods

Materials
Instantized cocoa beverage powders were
acquired from local superstores. Five different
brands from minor and major manufacturers
(Nestl, Vevey, Switzerland, Kraft Jacobs
Suchard, Bremen, Germany, and others) were
chosen for investigation. The products, labelled
A, B, C, D, E and F in the text below, contained
1920% low-fat cocoa, 2030% glucose and
5060% sucrose, as stated by the manufacturers.
All powders contained lecithin and, to our knowledge, all were instantized by agglomeration. For
comparison, beverage powders consisting of lowfat (12% fat) cocoa, lecithin (lecithin-cocoa ratio
1 : 19) and sucrose were mixed, milled and steam
jet agglomerated in the laboratory (for details on
steam jet agglomeration see Hogekamp et al.,
1996 and Hogekamp, 1997). A typical particle
size distribution of ground sucrose is shown in

Figure 1 Typical particle size

distribution for ground sucrose


approximated by the log-normal
type of distribution function
(MALVERN 2600c
measurement).

International Journal of Food Science and Technology 1999, 34, 335342

1999 Blackwell Science Ltd

Wetting behaviour of instantized cocoa P. Kyaw Hla & S. Hogekamp

Fig. 1. All PSDs of ground materials could be


described well by the log-normal type of distribution function with sln in the range of 0.70.8.
Methods of measurement
Wetting time
Since for most instantized beverage powders, the
wetting of the powder is the critical (i.e. rate controlling) step of the redispersing process, the wetting time of the powder samples was investigated
to characterize the instant behaviour. Since most
of the experiments were carried out with cocoa
beverage powders, milk at refrigerator temperature was used as testing liquid in most cases.
The wetting tester used for the measurements
(Hogekamp, 1997) consists of a 80 cm3 container
for the testing liquid and a powder sample section
which rests above the liquid container (see
Fig. 2). A slide, which is connected to a spring,
forms the bottom of the powder sample section.
Before each measurement, a powder sample of
approximately 8 g was prepared from bulk material (usually a 500 g or 800 g package). If desired,
screening was performed first, using 8 inch diameter analysis screens on a Retsch VE 1000
(Retsch, Haan, Germany) screening machine. A
sample dividing instrument (Fritsch laborette 27;
Fritsch, Idar-Oberstein, Germany) was then used
for representatively reducing the sample size to
the desired amount and the sample was placed in
the powder sample section of the wetting tester.
Secondly, the liquid (e.g. milk at 7 8C) was
poured into the liquid container and the powder
sample section was placed on top of the container. Unlocking the slide then let the spring quickly pull the slide out sideways, so that the powder
contacted the liquid after falling 23 mm, started
to wet and sink down into the liquid. The wetting

Figure 2 Schematic view of the wetting time testing

device.

1999 Blackwell Science Ltd

time, i.e. the time necessary for all the powder


particles to disappear, was recorded using a stopwatch. As it is generally difficult to determine
exactly the wetting time for slowly-wetting powders, each experiment was repeated at least three
times and the results were averaged.
Particle size
Particle size analysis was carried out for fine particles only (ground sucrose). A Malvern 2600c
(Malvern Instruments, Malvern, Worcestershire,
England) laser sizer equipped with a stirred liquid
sample cell was used in the measuring range
5.8 mm to 580 mm (300 mm Fourier lens) to get
the xv,0.5 value of the particle size distribution. The
sucrose particles were suspended in sucrose-saturated acetone.
The average particle size of the samples of
agglomerated material was simply calculated as
the arithmetic mean of the upper and lower
screen mesh size used for preparing the sample
from a portion of bulk powder.

Results

Preliminary tests
To get an impression of how different testing liquids might affect the wetting time, the wetting
time of a powder sample was tested using water
and milk of varied fat content. The wetting time
of powder A was tested with three different types
of UHT milk (i.e., 0.3%, 1.5%, 3.5% fat content)
and with deionized water (conductivity < 0.5 mS).
It was found that a higher fat content in the
milk leads to longer wetting times (7 min 47 sec,
9 min 7 sec and 11 min 3 sec, respectively). With
water the wetting time is much shorter (2 min 48
sec), as it contains no fat droplets, dissolved protein etc. Low-fat UHT milk (1.5% fat content)
appeared to be a good compromise testing liquid
for cocoa beverage powders and was used for all
further experiments.
To get a first impression of the dependency of
the wetting time of a fully soluble powder on the
average particle size, sucrose of different particle
size was investigated. The influence of adding a
non-wettable component like cocoa can also be
judged by comparing with these results. Crystal
sugar (sucrose) ground at different milling speeds

International Journal of Food Science and Technology 1999, 34, 335342

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Wetting behaviour of instantized cocoa P. Kyaw Hla & S. Hogekamp

Table 1 Wetting time of sugar

(sucrose) ground at different mill


speeds as a function of average
particle size

x50,3 /mm21
twet /sec21

in a rotor mill (Retsch SR3, Retsch, Haan,


Germany at 30, 36, 42, 48, 54 and 60 m sec21 circumferential velocity) was chosen for the experiments. After milling, the powder was stored
under vacuum for 24 h to allow recrystallisation.
In this experiment, it was found that the wetting
time decreased with increasing average particle
size. Reducing the average particle size from <
130 mm to < 40 mm increased the wetting time by
almost a factor of 20. The data and the respective
curve are shown in Table 1.
Influence of the removal of large
agglomerates from the powder
Breakage during handling and transport may
cause a loss of large-sized particles in an agglomerated product. Probability of breakage increases
with agglomerate size. It was therefore investigated how removing large particles from a powder
affects the wetting behaviour of the remaining
material. Samples of beverage powder C with a
particle size in the range from 0.1 mm to 1 mm

41.6
66.3

56.1
30.0

62.5
16.3

63.7
13.7

77.8
10.3

105.7
6.0

132.4
3.7

were chosen for the experiments. First, all particles above a given size were removed from the
sample by screening. Then, the wetting time of an
8 g sample of the remaining fines was tested.
In this experiment, it was found that removing
the larger particles had little influence for mesh
sizes between 0.28 mm and 1 mm. The wetting
time changed slightly from 7 to 13 sec. Carrying
out the experiment with particles below 0.2 mm
mesh size increased the wetting time to < 5 min.
Lowering the maximum particle size even further
increased the wetting time to almost 30 min, as
now the powder mainly consisted of fines plus
some very small agglomerates. The resulting wetting times are shown in Fig. 3.
Influence of ageing
The experiments described above were repeated
after the powder had been exposed to ambient
conditions in the open bag for one month. No
significant difference in wetting time could be
found for the fines , 0.2 mm, but the wetting

Figure 3 Wetting time of cocoa

beverage powder C as a function


of maximum particle size (larger
particles removed by screening)
for fresh material and for
material stored under ambient
conditions for one month.

International Journal of Food Science and Technology 1999, 34, 335342

1999 Blackwell Science Ltd

Wetting behaviour of instantized cocoa P. Kyaw Hla & S. Hogekamp

Figure 4 Wetting time of cocoa

beverage powder C as a function


of average particle size for
narrow fractions produced by
screening.

time for the larger fractions containing mostly


agglomerates had almost tripled (Fig. 3). The reasons for this kind of behaviour are still not understood. One cause may be migration of lecithin
away from the surface of the cocoa particles, but
transitions in the structure of the solid bonds
inside the agglomerates (from glassy to crystalline
state) may also be involved.

Influence of the average particle size of a


narrow agglomerate fraction
For low-fat milk powder and cocoa beverage
powders, earlier measurements (Schubert, 1993)
have shown a rapid rise of the wetting time for a
particle size below x < 150 mm. According to literature, this rapid rise is typical of many food

Figure 5 Wetting time of cocoa

beverage powder C mixtures consisting of fines (, 160 mm) and


agglomerates (0.45-0.56 mm) as a
function of the amount of fines.

1999 Blackwell Science Ltd

International Journal of Food Science and Technology 1999, 34, 335342

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Wetting behaviour of instantized cocoa P. Kyaw Hla & S. Hogekamp

products with particle size 3 ,160 mm to 200 mm


(Schubert, 1993). Samples of beverage powder C
of various average particle sizes between 0.113
mm and 1.13 mm were chosen for more detailed
experiments. Powder samples were prepared by
screening.
In this experiment, the average particle size had
only a small influence between 0.18 and 1.13 mm,
with wetting times between 3 and 8 sec. However,
at the average sizes of 0.14 and 0.11 mm, the wetting time increased to 3 and 23 min, respectively.
The relationship between wetting time and average particle size is shown in Fig. 4.
Influence of fines caused by abrasion of
agglomerates
In addition to breakage, agglomerated materials
may also develop a fines fraction caused by abrasion during transportation and handling. For
investigating the influence of the fines content in
a powder consisting of fines and agglomerates, a
fines fraction (, 0.16 mm) and an agglomerate
fraction (0.450.56 mm) were prepared from
cocoa beverage powder C by screening. Fines and
agglomerates were then mixed together in varied
proportion and the wetting time of these mixtures
was tested.

In this experiment, mixtures with higher content of fine particles showed longer wetting time.
The wetting time for mixtures with up to 40%
fines was between 13 and 15 sec. At higher fines
contents, the wetting time increased. In the mixture with a fines content of 60%, the wetting time
doubled to 30 sec. The resulting wetting times are
shown in Fig. 5.
Influence of the removal of fines from the
powder
In some cases, the instant properties of a powder
are adjusted by incorporating a screening step in a
production line to reduce the amount of fines
(which are then recirculated). Experimental work
on this subject (similar to that carried out above)
was carried out with cocoa beverage powder A.
This powder was separated into two fractions by
screening at 200 mm. Fines (, 200 mm) and
agglomerates (. 200 mm) in varied proportion
were then mixed together and the wetting time of
these mixtures was tested.
Again, it was found that for a higher content of
fine particles, the wetting time increased. For this
product, though, the behaviour was different, as
the wetting time increased continually with rising
amount of fines. A much wider range of wetting

Figure 6 Wetting time of cocoa

beverage powder A mixtures


consisting of fines (, 200 m)
and agglomerates (. 200 m) as
a function of the amount of fines.

International Journal of Food Science and Technology 1999, 34, 335342

1999 Blackwell Science Ltd

Wetting behaviour of instantized cocoa P. Kyaw Hla & S. Hogekamp

Figure 7 Wetting time of steam

jet agglomerated powder mixtures


consisting of sucrose and low-fat
lecithinated cocoa as a function
of the amount of cocoa.

times was measured (between 10 and 420 sec, see


Fig. 6).
Comparison between powders from different
manufacturers
Cocoa beverage powders of basically equal composition (e.g. < 20% cocoa, 20% glucose, 60%
sucrose) are available from many manufacturers.
Although never explicitly stated on the packages,
it is most likely that all these products are manufactured in different ways. Also, the type of cocoa
used, the amount of lecithin added and the method
of lecithination may vary from product to product.
All this may cause considerable variations of the
Table 2 Wetting time of instant cocoa beverage samples

instant behaviour of these basically similar


powders.
To eliminate the influence of the particle size
distribution on the wetting time, only narrow
agglomerate fractions (0.3550.45 mm) prepared
by screening were tested. Powders A, B, C, D, E
and F were chosen for a comparison and their wetting time was tested in low-fat milk of 7 8C.
Although some variation of the wetting time
had been expected, we were surprised to find
results extending from 6 sec to over 14 min. The
resulting wetting times are shown in Table 2.
Product E probably suffers from an unfavourable
agglomeration method, as ground powder of type
E, after steam jet agglomeration in our laboratory
plant, gave results comparable to the other products.

(trade products) in UHT milk (7 8C, 1.5% fat)


Product

Wetting time/s

A (all sizes)
A (355450 mm)
B (355450 mm)
C (all sizes)
C (355450 mm)
D (all sizes)
D (355450 mm)
E (all sizes)
E (355450 mm)
F (all sizes)
F (355450 mm)

167
11
47
7
6
37
13
840
425
38
15

1999 Blackwell Science Ltd

Influence of the cocoa content in a basic


cocoa/sugar mix
Cocoa beverage powders consisting only of ground
sucrose and low-fat, lecithinated cocoa (12% fat,
lecithin-cocoa ratio 1:19) were mixed and milled in
a rotor mill (Retsch SR3, Retsch, Haan, Germany)
at a circumferential velocity of 60 m sec21. Cocoa
content was varied from 0 to 30% wt/wt in steps
of 2 percent points. The milled powder samples
were then steam jet agglomerated (using a vibration feeder at very low feed rate to obtain a prod-

International Journal of Food Science and Technology 1999, 34, 335342

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Wetting behaviour of instantized cocoa P. Kyaw Hla & S. Hogekamp

uct free of fines) and the wetting time measured in


UHT milk (1.5% fat, 7 8C).
The results show an interesting relation between
cocoa content and wetting time (Fig. 7): from 0 to
< 25% cocoa, the wetting time rises continually
but slowly (from < 1 to < 7 s), while for higher
cocoa contents, the wetting time increases much
more rapidly. It is obviously much more difficult
to produce instantized cocoa beverage powders
with 30% cocoa instead of 20% and have good
wetting behaviour (although a few products of this
type are on the market).

fines is generally unpopular. A well-instantized


powder may tolerate a certain amount of fines
developing, for example, by abrasion during transportation.
Exposure to air after opening the sealed package
led to reduced wettability over time. After a period of one month, wetting time may be three times
as long as for the fresh powder. There is evidently
still need for improvements by all manufacturers
regarding long-time stability of instant properties.

Acknowledgements
Conclusions

The products investigated in this work showed a


wide variation regarding their wettability, although
their composition and manufacturing method were
quite similar. It seems that agglomeration problems like excessive fines content or unfavourable
agglomerate structure are the main cause for insufficient wettability, while the cocoa content, for
example, seems to be less important.
The experiments showed that it is not so much
the production of large agglomerates but rather
the removal of fines that makes a powder wet easily. The critical particle size below which as few
particles as possible should appear in the final
product lies around 180 m, with a product-dependent margin of approximately 6 20 mm. Screening
may improve the quality of an insufficiently
agglomerated powder, although recirculation of

The authors wish to thank the DAAD (Deutscher


akademischer Austauschdienst) for the financial
support of this research work. Mrs P. Kyaw Hla
furthermore wishes to express her gratitude to the
staff of the Institute of Food Process Engineering
for their help.

References
Hogekamp, S. (1997). ber eine modifizierte
Strahlagglomerationsanlage zur Herstellung schnell
dispergierbarer Pulver. Dissertation, Universitt
Karlsruhe.
Hogekamp, S., Schubert, H. & Wolf, S. (1996). Steam jet
agglomeration of water soluble material. Powder
Technology, 86, 4957.
Schubert, H. (1979). Grundlagen des Agglomerierens.
Chemie Ingenieur Technik, 51, 266277.
Schubert, H. (1993). Instantization of powdered foods.
International Chemical Engineering, 30, 2845.

International Journal of Food Science and Technology 1999, 34, 335342

1999 Blackwell Science Ltd

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