food and bioproducts processing 9 0 ( 2 0 1 2 ) 406412

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Food and Bioproducts Processing

journal homepage: www.elsevier.com/locate/fbp

Effect of initial dextrose concentration, seeding and cooling

prole on the crystallization of dextrose monohydrate
Abhay Markande a,d , John Fitzpatrick a, , Amale Nezzal b , Luc Aerts c,d , Andreas Redl d
a

Department of Process and Chemical Engineering, University College Cork, Cork, Ireland
Nezzal Powder Consulting, 55 rue Bermond, 81000 Albi, France
c UCB Pharma, Avenue de lIndustrie, Braine lAlleud, Belgium
d Innovation Center, Syral N.V., Aalst, Belgium
b

a b s t r a c t
A batch seeded cooling crystallizer was used to study dextrose monohydrate crystallization. Experiments were conducted to investigate how a 2% increase in the initial dextrose concentration (from 65.5 to 67.5%) would inuence
nal crystal yield and size. The crystallizations were performed for three different seed masses and cooling proles,
consequently the inuence of these parameters was also investigated. The parameters were varied in accordance
with an industrial scale process. An in-line focused beam reectance measurement probe and an in-line process
refractometer were used to continuously monitor the crystallizations. The experimental results showed that the 2%
increase in initial dextrose concentration had a major inuence on the rate of crystallization and yield over a 24 h
crystallization period, and only a minor inuence on the median crystal size.
2011 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
Keywords: Crystallization; Dextrose

1.

Introduction

Industrial scale continuous crystallizers often exhibit periodic changes of supersaturation, solid phase content, crystal
size, and production rate. In continuous crystallizers, crystal
size distribution deviates from the desired distribution due to
the presence of external disturbances, such as changes in the
concentration of solute in the feed stream, and due to the randomly occurring changes in the operating conditions. In batch
processes, batch crystallizer suffers from a changing level of
supersaturation during their operation.
In sugar manufacturing, dextrose monohydrate is produced by crystallization of high dextrose equivalent (DE)
syrup. At the start of crystallization, the syrup is seeded with
massecuite from a previous batch. The massecuite is a slurry
containing grown crystals suspended in the syrup at the end of
crystallization. During production, the mixing ratio of massecuite to syrup is often varied and hence the concentration of
dextrose at the start of crystallization process changes. The
increase or decrease in initial dextrose concentration may
inuence the crystallization rate and yield of the process as

well as the nal crystal size distribution resulting from nucleation and growth phenomena. In relation to the dextrose
crystallization, the amount of crystals produced is very sensitive to variations in the initial dextrose concentration and the
temperature prole (Parisi et al., 2007).
A key variable during batch crystallization processes is the
solution supersaturation which signicantly determines the
development of nucleation and growth phenomenona (Srisanga et al., 2006) and consequently, the nal crystal yield and
size. It is well established that the rate of cooling directly
affects both nucleation and growth kinetics. For instance, a
fast cooling regime results in the build-up of supersaturation to levels that have preference for nucleation over growth,
consequently leading to a large population of smaller sized
crystals. On the other hand, a controlled cooling regime can
control supersaturation so as to grow the nucleated crystals
rather than produce new nuclei, resulting in larger sized crystals (Jones and Mullin, 1974). Besides, Kubota et al. (2001)
showed that seeding plays a key role in crystallization to
control crystal size distribution (CSD). If the seed mass is insufcient, then secondary nucleation will be important and the

Corresponding author.
E-mail address: j.tzpatrick@ucc.ie (J. Fitzpatrick).
Received 16 February 2011; Received in revised form 25 August 2011; Accepted 23 November 2011
0960-3085/$ see front matter 2011 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
doi:10.1016/j.fbp.2011.11.010

407

food and bioproducts processing 9 0 ( 2 0 1 2 ) 406412

nal CSD will be dispersed. On the other hand, a large quantity

of seeds reduces productivity (Doki et al., 2001). Overall minor
changes in these crystallization parameters can produce signicant changes in crystal yield and size.
In-line monitoring can be applied in trying to interpret how
changes in process variables inuence the performance of
a crystalliser. For example in a batch crystallization, in-line
monitoring can be applied to measure the component concentration in solution and CSD continuously over time. This
can be applied to investigate how process parameters, such as
seed size or cooling rate, inuence the nal crystal yield and
nal CSD. In sugar crystallization, the sugar concentration in
the mother liquor can be estimated by measuring the refractive index of the sugar slurry as a whole since the presence of
crystals hardly affects the measurement. The refractive index
measurement is used to give the brix, from which the total
dissolved solids content can be evaluated. If the initial purity
of the syrup is known then the sugar concentration can be
evaluated. In line process refractometers exist to measure the
refractive index continuously, such as the K-Patents process
refractometer. Focus beam reectance measurement (FBRM)
has emerged as a widely used technique for the in situ particle size characterization of high-concentration particulate
slurries, such as occur in many crystallizations. FBRM is a
probe based measurement, which is installed directly in the
crystallizer without the need for sample dilution or manipulation (Barrett and Glennon, 1999). FBRM has been successfully
applied as a useful tool for detecting nucleation and characterizing the metastable zone width (Barrett and Glennon, 2002).
FBRM measures a chord length distribution, which can be
related to a particle size distribution (Worlitschek et al., 2005).
Secondary nucleation and particle growth can be attributed
to the time evolution of chord length distribution (Kail et al.,
2009). Markande et al. (2009) utilized an in-line K-Patents
refractometer and a FBRM probe to investigate the inuence of
seeding and cooling prole on the crystallization of dextrose
monohydrate with an initial dextrose concentration of 65.5%.
As already stated above, dextrose crystallization is very
sensitive to variations in the initial dextrose concentration
and the temperature prole. At an industrial scale, uctuations in initial dextrose concentrations do occur, consequently
the main objective of this paper was to investigate how a typical range of variation in initial dextrose concentration (i.e.
from 65.5% to 67.5%) inuences the nal dextrose crystal yield
and size, and rate of progression of the crystallization. Inline K-Patents refractometer and FBRM probe, as described
by Markande et al. (2009), were used during the experimentation. This experimentation was carried out for three different
seed masses and cooling proles, consequently, the inuence
of these parameters was also investigated. Furthermore, the
in-line measurements provided data throughout the crystallizations (and not just at the beginning and end) and these
data were used to help in the interpretation of the results.

2.

Materials and methods

2.1.
Dextrose monohydrate seed crystals and dextrose
syrups
d-glucose, commercially known as dextrose, can be crystallized to either anhydrous or hydrate form from an aqueous
solution. It has three different crystal forms: monohydrate,
anhydrous and anhydrous dextrose. In this work, the studied

Table 1 Dry substance composition of dextrose syrup

by HPLC.
Component

% (w/w)

Dextrose
Maltose
Maltotriose
Higher sugars
Others (fructose)

93.3
3.62
1.62
1.29
0.17

crystalline dextrose is the dextrose monohydrate (DMH) form.

The seeds of dextrose monohydrate crystals of 99.5% purity
were supplied by Syral Belgium N.V., Belgium as industrial
grade quality. The seeds were in a size range of 125150 m,
as measured by sieve analysis.
Dextrose monohydrate was produced by crystallization of
high dextrose equivalent (DE) syrup. Two syrups were supplied
by Syral Belgium N.V., Belgium, having dextrose concentrations of 65.5% and 67.5%. Dextrose concentration is dened as
mass of dextrose per unit mass of solution excluding impurities. Both syrups had the same purity of 93.3% (w/w of total
sugar), as measured by HPLC, and the dry substance composition of the syrup is presented in Table 1.

2.2.
Experimental set up for in-line monitoring of the
batch crystallizer
The batch cooling crystallization experiments were performed
in a 3.2 L jacketed glass crystallizer with a U-shaped bottom.
The diameter of the crystallizer was 150 mm with a height of
200 mm. The batch vessel was equipped with an anchor type
agitator. The agitator of diameter 100 mm, height 60 mm and
width 22 mm was used. An agitator was placed at a height
15 mm from the bottom of the crystallizer. All experiments
were performed at 38 rpm to ensure all the crystals were maintained in suspension. The temperature in the crystallizer was
controlled with a programmable thermostat. A constant batch
size of 2 kg of slurry was used in all experiments.
The set up was equipped with two in-line measurement
instruments. A K-Patents process refractometer (K-Patents PR23-AP) and a FBRM D600 probe were used to monitor the liquid
phase and chord length distribution, respectively. The position
of the probes was chosen in the high mixing zone, i.e. near the
agitator. The measurements from both probes were recorded
every 2 min. As the measurement by FBRM and in-line refractometer change in a continuous way, the data at every 1 h is
considered for the comparison. The complete experimental
setup used in this study is shown in Fig. 1.

2.3.

Evaluation of yield of crystals produced

The yield is dened as the mass of dextrose crystals produced

during a crystallization trial divided by the mass of dextrose in
solution at the beginning of the trial. This is expressed mathematically in Eq. (1).
Yield =

MC
MF Cd0

(1)

where MC is the mass of crystals produced during crystallization, MF is the mass of feed solution and Cd0 is the initial
dextrose concentration in solution at the beginning of the
crystallization (expressed as a mass fraction). Both MF and Cd0
exclude the small amount of impurities present.

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food and bioproducts processing 9 0 ( 2 0 1 2 ) 406412

Fig. 1 Experimental batch crystallization set-up.

The K-Patents in-line refractometer was used in the evaluation of dextrose concentration over time, including the initial
concentration and the nal concentration at the end of a crystallization trial. The refractometer measures refractive index
as a Brix value and this was converted to dextrose concentration using a calibration table (details of this procedure are
provided in Markande, 2009). Once again, the dextrose concentrations are expressed as mass of dextrose per unit mass
of solution excluding impurities.
The evaluated nal dextrose concentration (CdF ), expressed
as a mass fraction, was used to calculate the mass of crystals
using the following Eq. (2).

In this work, yields obtained from 67.5% initial dextrose concentration trials (Yield67.5% ) is compared with those
from corresponding 65.5% initial dextrose concentration trials
(Yield65.5% ). In addition to comparing the difference in yields,
the percentage increase in yield of the 67.5% trials over the corresponding 65.5% trials is presented. This percentage increase
in yield is dened in Eq. (4).
% Increase in yield = 100

2.4.
MF (Cd0 CdE )
MC =
1 CdE

(2)

Substituting Eq. (2) into Eq. (1) and expressing yield as a percentage gives Eq. (3), and this equation was used to calculate
yields.
Yield = 100

(Cd0 CdE )
(1 CdE )Cd0

(3)

Controlled cooling

Crystallizations were performed by cooling down the seeded

syrup from 42 C to 33 C in 24 h. During the crystallization
trials, seeding was performed at 42 C. Crystallization trials
were performed at each of the initial dextrose concentrations
of 65.5% and 67.5% for three seed masses of 5%, 12.5% and
20% and three cooling proles. The cooling proles used were
either natural, linear or controlled (illustrated in Fig. 2) as given
by the following temperature (T)time (t) relationship in Eq. (5).

 n
t
tf

(5)

Linear cooling

42

Temperature( C)

(4)

Batch cooling crystallizations

T(t) Ti
=
Tf Ti

44

Yield67.5% Yield65.5%
Yield65.5%

where n = 1 is linear; n = 3 is controlled and n = 1/3 is natural

(subscripts i and f are initial and nal, respectively).

Natural cooling

40
38

Table 2 Crystal yield for duplicate trials.

Cooling prole

36
34

Initial dextrose
concentration
(kg/kg)

32
0

10

12

14

16

18

20

22

24

Time (hrs)
Fig. 2 Cooling proles used in batch crystallizations.

26

Linear
Linear
Natural

65.5
67.5
67.5

Crystal yield (%)

Trial 1

Trial 2

22.89
32.82
36.19

23.00
33.06
36.85

409

18

69

15

67

12
9
6
3
0
1

10

100

1000

Dextrose Concentration (%)

Number frequency (%/micron)

food and bioproducts processing 9 0 ( 2 0 1 2 ) 406412

65
63
61
59
57

Chord length (microns)

55

Fig. 3 Comparison of duplicate frequency chord length

distributions (linear cooling prole; 12.5% seed mass).
The reproducibility of the in-line monitoring techniques
and the crystallization procedure was assessed by performing duplicate trials with linear and natural cooling proles
and two initial dextrose concentrations. Comparison of crystal yield obtained for each of the duplicate trials is presented
in Table 2 and a comparison of the chord length distribution
for one of the duplicate trials is presented in Fig. 3.

at 67.5% dextrose concentration

at 65.5% dextrose concentration
Solubility curve

30

32

34

36

(a)

Crystallizations were performed at the two initial dextrose

concentrations of 65.5% and 67.5%. With a difference of only
2% between the two concentrations it may intuitively be
expected that there may not be much difference between
the crystallizations, however it does depend on the solubility diagram and the solubility at the temperature at the end of
crystallization in particular. This temperature was 33 C and
the corresponding dextrose solubility is 0.568 g dextrose per g
of solution or 56.8% (Markande, 2009). The maximum yield for
each of the initial concentrations can be obtained by applying Eq. (3) with a nal dextrose concentration equal to the
solubility limit. From this, the maximum yields for the initial concentrations of 65.5% and 67.5% were 30.8% and 36.8%,
respectively. Consequently, the 2% variation in initial dextrose
concentration leads to a 6% difference in yield of the 67.5% trial
over the 65.5% trial, if equilibrium were to be achieved at the
end of crystallization. Expressing this as a percentage increase
in yield (Eq. (4)), this represents a 19.5% increase in yield.
Furthermore, the difference in initial concentration may
affect the rate of progression of the crystallization. The higher
concentration may be expected to take longer because there is
more dextrose in solution, however the higher initial supersaturation may counteract this. Overall, it is intuitively difcult
to predict what may happen.
Fig. 4 displays a comparison of the soluble dextrose concentration temperature proles for two trials carried out
at 65.5% and 67.5% initial dextrose concentration. Both trials
were performed with a natural prole and at 5% seed mass.
The rate of crystallization is faster at the higher initial dextrose
concentration of 67.5% resulting in the nal soluble dextrose
concentration at the end of crystallization being lower for the
67.5% trial. The corresponding yields for the 65.5% and 67.5%
trials were 26% and 36%, respectively. This is a major difference but it needs to be considered in the context of the
maximum yields of 30.8% and 36.8% for the 65.5% and 67.5%

Supersaturation

3.1.
Effect of initial dextrose concentration on the
crystallization

42

44

1.35
at 65.5% dextrose concentration
at 67.5% dextrose concentration

1.25
1.20
1.15
1.10
1.05
1.00
0

10 12 14 16 18 20 22 24 26

Time(hrs)

(b)
2.2.E+04

Particle counts (#/sec)

Results and discussion

40

Fig. 4 Effect of initial dextrose concentration on the

soluble dextrose concentrationtemperature prole (both
trials were performed with a natural cooling prole and at
5% seed mass).

1.30

3.

38

Temperature (C)

Particle counts of 1-112 m

2.0.E+04
1.8.E+04
1.6.E+04
1.4.E+04
1.2.E+04
1.0.E+04

Natural cooling at 65.5% concentration

Natural cooling at 67.5% concentration

8.0.E+03
6.0.E+03
0

10 12

14

16

18 20

22

24

26

Time (hrs)

Fig. 5 Time evolution of (a) supersaturation and (b) FBRM

counts per second in the 1112 m size range during
crystallization (natural cooling prole; 5% seed mass).
trials, respectively. The 67.5% trial is near its maximum of
36.8% and is thus near equilibrium.
The in-line measurements of dextrose concentration and
chord length distribution (CLD) taken throughout the crystallization can be used to interpret the rate of crystallization
progression in both trials. Converting the dextrose concentration data into how supersaturation varies with time is
presented in Fig. 5a. Fig. 5b shows the corresponding FBRM
counts per second data in the size range from 1 to 112 m.
As this is below the size of the seeds, these data are used
as an indicator of the generation of nuclei. It is important
to note that in a chord length distribution the number of
shorter chords does not directly correspond to the number of
the smaller crystals. For example, a short chord can be also

food and bioproducts processing 9 0 ( 2 0 1 2 ) 406412

3.2.
yield

Effect of initial dextrose concentration on crystal

Further trials were undertaken to investigate how the change

in initial dextrose concentration from 65.5 to 67.5% inuenced crystallizations performed with the three different seed
masses (5%, 12.5%, 20%) and three different cooling proles
(linear, natural, controlled). The results from these trials are
presented in Table 3. It is clearly observed from Table 3 that
the 2% change in initial dextrose concentration strongly inuenced the yield of the process. For example, during natural
cooling at 67.5% concentration, the percentage increase in
yields (Eq. (4)) were 38%, 33%, and 24% for the 5%, 12.5%, and
20% seed masses, respectively. In the case of linear cooling,
the percentage increase in yields were larger at 55%, 43% and
34% for the 5%, 12.5 and 20% seed masses, respectively. However, this must be considered in the context of an inherent
19.5% increase in yield that would be obtained if equilibrium
was achieved by both 67.5% and 65.5% initial dextrose concentration trials. Consequently, the higher yields were in-part
obtained by both the faster rate of crystallization during the
24 h crystallization period and the inherent higher maximum
equilibrium yield obtainable by the higher initial dextrose concentration trials.

Particle counts (#/sec)

45
Particle counts of 194-233 m

40
35
30
25
20
15
10
5

Particle counts (#/sec)

0
2.2.E+04
Particle counts of 1-112 m

2.0.E+04
1.8.E+04
1.6.E+04
1.4.E+04
1.2.E+04
1.0.E+04

Natural cooling at 65.5% concentration

Natural cooling at 67.5% concentration

8.0.E+03
6.0.E+03
0

Effect of initial dextrose concentration on crystal

Even though a major increase in yield was observed at

higher initial dextrose concentration, there was little inuence
observed on the nal median crystal size (Table 3). A decrease
in crystal size at 5% seed mass was observed during natural
cooling. However, at 5% seed mass, linear and controlled cooling showed an increase in crystal size. The nal crystal size at
12.5% and 20% showed no signicant inuence upon change in
the initial dextrose concentration. In fact, it might be expected
that the higher dextrose consumption would produce larger
crystals. Actually, despite the high dextrose consumption and
the increase in solid concentration, the additional crystal mass
produced was due to the newly generated crystals and their
subsequent growth.

10

12

14

16

18

20

22

24

26

Fig. 6 Comparison of particle counts in the 1112 m and

194233 m size ranges for natural cooling (5% seed mass
and initial dextrose concentrations of 65.5% and 67.5%).
45
Particle counts of 194-233 m
40
35
30
25
20
15
10
5
0
2.2.E+04
Particle counts of 1-112 m

2.0.E+04
1.8.E+04
1.6.E+04
1.4.E+04
1.2.E+04
1.0.E+04

Linear cooling at 65.5% concentration

Linear cooling at 67.5% concentration

8.0.E+03
6.0.E+03
0

3.3.
size

Time (hrs)

Particle counts (#/sec)

generated by a larger crystal if the beam intersects it close to

its border (Worlitschek et al., 2005). Furthermore, the chords
in the range of 1112 m can be also generated by the seeds,
however, if the number of the shorter chords increases during
the crystallization, the increase can be used as an indicator of
nucleation.
For the higher initial dextrose concentration of 67.5%,
Fig. 5a shows the highest increase in supersaturation at
around 6 h, after which there is a very rapid decrease in
supersaturation. The particle counts data in Fig. 5b shows the
highest counts for the higher initial dextrose concentration of
67.5%, inferring that the highest levels of nucleation occurred
during this trial. One explanation for the higher nucleation
observed in the 67.5% trial is that the higher levels of supersaturation caused higher levels of secondary nucleation (as
opposed to primary nucleation as these levels are still within
the metastable zone for dextrose monohydrate). The high
levels of nucleation created many new crystals which greatly
increased the surface area available for crystal growth and
it is this additional crystal surface area that resulted in the
increased crystallization rate and rapid reduction of dextrose
in solution.

Particle counts (#/sec)

410

10

12

14

16

18

20

22

24

26

Time (hrs)

Fig. 7 Comparison of particle counts in the 1112 m and

194233 m size ranges for linear cooling (5% seed mass
and initial dextrose concentrations of 65.5% and 67.5%).
FBRM chord length data for natural and linear cooling proles are presented in Figs. 6 and 7, respectively. Both show a
more rapid increase in the counts measured in the 1112 m
range for the 67.5% concentration. The high increase of particle counts of 1122 m at 67.7% concentration indicates high
nuclei formation through secondary nucleation. As already
mentioned, the secondary nucleation may be caused by the
higher levels of supersaturation, however this may not necessarily be the only dominant mechanism. For example, there
is also the possible inuence of secondary nucleation by the

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food and bioproducts processing 9 0 ( 2 0 1 2 ) 406412

Table 3 Effect of initial dextrose concentration, seed mass and cooling prole on crystal yield and size.
Cooling

Seed mass (%)

D50
Natural
Natural
Natural
Linear
Linear
Linear
Controlled
Controlled
Controlled
a

5
12.5
20
5
12.5
20
5
12.5
20

Concentration 67.5%(%)

Concentration
65.5 (%)
1

Yield

144
130
121
134
131
122
129
126
107

D50

26
27
29
20
23
26
11
19
21

129
130
122
149
129
123
146
128
121

Yield
36
36
36
31
33
35
23
28
31

Median chord length in m.

collision mechanism, where the magma density plays a major

role in the nucleation rate (Myerson and Ginde, 2002).
For the natural cooling prole, Fig. 6 shows that the increase
in larger crystals (194233 m particle counts) at 67.7% concentration was lower than at 65.5% concentration. A high amount
of ne crystals (1112 m particle counts) generated and a
slow asymptotic increase in larger crystals at 67.5% dextrose
concentration resulted in a lower median crystal size. The
same behaviour was observed at higher seed masses (data
not shown) for the natural cooling prole giving an increase in
ne counts with increased dextrose concentration, although,
there was no signicant difference in the counts measured for
194233 m. The observed asymptotic increase in the longer
chord counts suggests that the number density of larger crystals does not increase at the higher magma densities. This may
be due to secondary nucleation by collision mechanism, where
the magma density plays a dominant role in the nucleation
rate (Myerson and Ginde, 2002). Since the collision mechanism
induces crystal breakage and a reduction of larger crystals, this
may offset their growth rate.
During linear cooling, the inuence of initial dextrose
concentration on the large particle counts (194233 m) was
different. For example, at 5% seed mass, Fig. 7 shows that the
large counts observed were greater at the 67.5% initial dextrose
concentration and this resulted in a larger median particle
size.
Comparing both sets of trials, the higher initial dextrose
concentration resulted in more ne crystals being produced
in the 1112 m range. This demonstrated the formation of
a higher number of nuclei, which is true for each of the
three cooling proles and seed masses. This produced an
increase in crystal surface area which increased the rate of
dextrose consumption. There was no clear trend observed
between the initial dextrose concentration and the large particle counts in the 194233 m range, with lower counts being
recorded for natural cooing at the higher dextrose concentration and the opposite occurring during linear cooling. The
lower counts during natural cooling may be explained by the
greater dominance of secondary nucleation, with more nuclei
being produced leading to smaller nal crystal sizes.

3.4.
Effect of seed mass and cooling prole on yield
and crystal size
Table 3 also shows the inuence of seed mass and cooling prole on yield and crystal size. Increasing seed mass caused an
increase in yield. This trend would be expected, as a greater

amount of seeds leads to higher crystallization rates during

the 24 h trials. Cooling prole also inuenced crystal yield with
the natural prole providing the highest yields and the controlled prole providing the lowest for both initial dextrose
concentrations. This is due to the higher crystallization rates
occurring during the natural cooling prole over the 24 h trials.
The inuence of seed mass and cooling prole on crystal
median size is less clear, although lower seed mass appears to
produce larger median crystal sizes. Markande et al. (2009) discusses these trends in more detail for the lower initial dextrose
concentration. Overall, Table 3 demonstrates the important
inuence of the initial dextrose concentration on yield during the 24 h trials, where the yields obtained for the 67.5%
initial dextrose concentration were consistently much higher,
irrespective of the seed mass and cooling prole used.

4.

Conclusions

The initial dextrose concentration of the inlet stream entering an industrial continuous crystallizer can uctuate and
this can inuence the performance of dextrose crystallization.
This paper investigated the inuence of a typical industrial
variation in initial dextrose concentration and how it affected
the rate of progression of the crystallization, crystal yield and
nal crystal size in a batch cooling crystallizer. The crystallization trials showed that a 2% increase in initial dextrose
concentration showed a signicant increase in dextrose crystal yield, with percentage increase in yields ranging from about
24% to 55% for the seed masses and cooling proles tested.
The main contributor to the increased percentage yields is
the inherent higher percentage increase in equilibrium yield
of 19.5% obtainable by the higher initial dextrose concentration. The remainder is due to faster crystallization rates being
achieved during the higher concentration trials, moving these
trials closer to equilibrium by the end of the 24 h crystallization
time.
In-line measurements were applied to continuously monitor and help interpret the crystallizations. Higher levels of
supersaturation were observed during the higher initial dextrose concentration trials using data obtained from the in-line
refractometer. The higher supersaturation levels led to greater
levels of nucleation, as monitored by the in-line FBRM probe.
The greater nucleation caused an increased rate of dextrose
consumption due to increased crystal surface area.
Both seed mass and cooling prole inuenced the rate
of crystallization at both initial dextrose concentrations. As
expected, higher seed mass resulted in faster crystallizations.

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food and bioproducts processing 9 0 ( 2 0 1 2 ) 406412

The natural cooling prole trials were the fastest while the
controlled cooling prole trials were the slowest for both initial
dextrose concentrations.
Contrary to the expectation that the higher dextrose consumption, at the higher initial dextrose concentration, would
produce larger crystals, there was little inuence observed on
the nal median crystal size. This is an indication of the importance of secondary nucleation and how it inuences nal
crystal sizes. Secondary nucleation was greater at the higher
initial dextrose trials which counteracted the greater dextrose
consumption, as the crystal mass produced was mainly due to
newly generated crystals and their subsequent growth. Overall, the crystal yields obtained and the amount of crystals
produced were very sensitive to variations in the initial dextrose concentration.

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