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Chemical Engineering and Processing 47 (2008) 21572162

Kinetics of the xylitol crystallization in hydro-alcoholic solution

Ernesto Acosta Martnez a,b,, Marco Giulietti c,d, Joao Batista de Almeida e Silva b, Silas Derenzo c
a

Cuban Institute for Research on Sugarcane Derivatives, P.O. Box 4026, Havana, Cuba
Lorena Engineering School, University of Sao Paulo, C. Postal 116, CEP 12602-810, Lorena, SP, Brazil
c Institute for Technological Research of S
ao Paulo, P.O. Box 0141, CEP 01064-970, SP, Brazil
d Federal University of S
ao Carlos, SP, Brazil
Received 26 March 2007; received in revised form 8 November 2007; accepted 9 November 2007
Available online 17 November 2007

Abstract
Nyvlt method was used to determine the kinetic parameters of commercial xylitol in ethanol:water (50:50 %w/w) solution by batch cooling
crystallization. The kinetic exponents (n, g and m) and the system kinetic constant (BN ) were determined. Model experiments were carried out
in order to verify the combined effects of saturation temperatures (40, 50 and 60 C) and cooling rates (0.10, 0.25 and 0.50 C/min) on these
parameters. The fitting between experimental and calculated crystal sizes has 11.30% mean deviation.
2007 Elsevier B.V. All rights reserved.
Keywords: Xylitol; Crystallization; Kinetics; Growth; Nucleation

1. Introduction
Xylitol is a polyol traditionally used by food and pharmaceutical industries as sucrose substitute for people with diabetics
and obesity, preventing dental caries and middle ear infections
in young children [1,2]. This sugar is commercially obtained
by a chemical process based on the reduction of xylose derived
mainly from wood hydrolysates [3].
Although most part of xylitol production studies are focused
on the hydrolysate treatment (pH alteration, ion-exchange resins,
active charcoal) and on xylose fermentation (pH, aeration, temperature, substrate concentration) [48], recent studies on xylitol
crystallization process are cited in the literature [913].
Xylitol has been crystallized from a highly concentrated solution containing xylose, arabinose, mannitol, arabitol, sorbitol
and other not detectable compounds [13,14].
Crystallization is a separation technique that has been used
for centuries and is often critical because it largely determines
the product purity and the handling characteristics such as
caking and wetting [11,15]. The separation step of the product can be one of the most significant operational costs of
the process. The material production with the desired quality

Corresponding author. Tel.: +551231595007.

E-mail address: ernesto.amartinez@yahoo.com.br (E.A. Martnez).

0255-2701/$ see front matter 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.cep.2007.11.004

often requires the knowledge of elementary steps involved in

the process such as creation of supersaturation, crystal nucleation and growth, aggregation and other secondary processes
[1517].
The choice of a crystallization method (cooling, evaporation, precipitation and salting-out) is dependent on the solubility
and saturation slopes with the temperature. Firstly, there is a
metastable zone where excess solute of the equilibrium concentration is deposited on existing crystals but no new crystal
nucleus is formed. Secondly, there is an intermediate zone
where both crystals growth and nucleation occur simultaneously.
Thirdly, there is a labile zone where nuclei are formed spontaneously from a clear solution. These three zones are controlled
not only by equilibrium, but also by process parameters like
agitation, temperature, solution purity and cooling rate. In order
to obtain a good product, the cooling rate must maintain the
supersaturation inside the metastable zone, thus minimizing the
formation of new crystals [16].
The kinetics of nucleation, growth and secondary nucleation
can be studied using model experiments in laboratory or pilot
plant and in continuous or batch processes. In batch mode,
nucleation and growth kinetic parameters can be derived by
monitoring, at least, supersaturation or crystal size distribution (CSD) and ideally both [18,19]. The average growth and
nucleation kinetics can be obtained when the CSD variable is
monitored at the end of the run [20]. In this case more than three

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E.A. Martnez et al. / Chemical Engineering and Processing 47 (2008) 21572162

experiments at varying batch time or average supersaturation are

needed [21].
The aim of this work is to investigate the combined effects
of saturation temperature and cooling rate on crystal size and
kinetics parameters of the xylitol crystallization process in
hydro-alcoholic solution using model experiments.
2. Materials and methods
2.1. Crystallization of xylitol
The xylitol crystallization experiments in waterethanol
(5050%, w/w) mixture were carried out according to the
methodology described by Martnez et al. [13]. Initially the
temperature of the solution containing xylitol and water was
raised to 10 C more than the saturation temperature, and maintained at this value for 5 min to ensure total solubilization of
xylitol. Subsequently, the solution was cooled at 2 C/min rate
until the saturation temperature and when reached the saturation
temperature (Tsat ) ethanol (99.7% at Tsat ) was added and the
solution was cooled. Four xylitol crystals (0.000250.00059 m)
were added when the solution temperature was 2.5 C lower than
the saturation temperature.
The solution was cooled at linear cooling rate (CR) using
a LAUDA RC6CP, GMBH & Co thermostatic bath, and the
WINTHERM Plus software, version 1.01. The nucleation temperature was defined by the turbidity alteration, when many
crystals were formed, and by the temperature versus time curve,
when the solution temperature increased. The software registers the values for suspension, set-point and thermostatic bath
temperatures as a function of time. Table 1 presents values of
saturation temperatures (Tsat ), linear cooling rates (CR) and the
solubility data determined by Vyglazov and Kholkin [11].
The experiments were carried out in a 100 mL glass jacketed
crystallizer with a type-helix agitator. The solution was stirred
with a IKA Labortechnic, RW 20.n agitator at 450 rpm. The
suspension was filtered in a Buchner funnel (125 cm diameter),
using Whatman filter paper, mark 42 for the retention of fine
crystals at the end of each experiment. The crystals were washed
with 100 mL ethanol (99.7 %) and dried under vacuum at room
temperature during 24 h. Once dried, the crystals were weighed
Table 1
Values of saturation temperature (Tsat ) and linear cooling rate (CR), xylitol and
waterethanol used in each model experiment (Vyglazov and Kholkin [11])
Tsat ( C)

CR
( C/min)

Experiment

Xylitol (g/100 g
solution)

Waterethanol
(g)

40

0.10
0.25
0.50

1, 2, 3
4, 5, 6
7, 8, 9

52.98

47.02

50

0.10
0.25
0.50

10, 11, 12
13, 14, 15
16, 17, 18

63.59

36.41

60

0.10
0.25
0.50

19, 20, 21
22, 23, 24
25, 26, 27

73.45

26.55

in Mettler Toledo PB 1502 balance, Sweden. All experiments

were performed in triplicate.
2.2. Analytical methods
The crystal size distribution (CDS) for each experiment
was obtained by sieving using Granustest, Talestem trademark Peneiras for Analises Ltda, with the following Mesh
(in m): 0.000106, 0.000177, 0.000250, 0.000590, 0.000710,
0.001, 0.00119, 0.00141, 0.00168 and 0.002. The crystals were
weighed using a Mettler Toledo PB 1502 balance.
The kinetics parameters were determined according to Nyvlt
methodology using M(L) and z as a function of crystal size. Thus
the mean size of each granulometric distribution was obtained
[20]. The mathematical model is based on kinetics equations of
nucleation and crystal growth, mass balance, gamma function
and distribution mean size. The crystals agglomeration and break
were inserted in the kinetic of growth and nucleation, respectively. So, the evaluated growth rate is apparent (non-linear).
The melting heat (259.66 J/g), melting point (93.61 C) and
purity (99.8%) of the xylitol crystal were determined by differential scanning calorimetry in a DSC822e, Mettler Toledo,
Sweden, using a STARe software.
The densities of solid xylitol and hydro-alcoholic mixture
were 1500 and 910 kg/m3 , respectively, and the crystal volume
shape factor was 0.83, as reported by Fernandes et al. [14].
The moisture of the xylitol crystal (0.05%) was determined
in Karl Fischer titrimeter, Mettler Toledo DL38, Switzerland.
3. Results and discussion
The nucleation kinetics is usually described by a common
power law:
B =

dN
= kN Mcc (C Csat )n
dt

it holds for the growth kinetics:



kG
dL
(C Csat )g
=
G=
dt
3c

(1)

(2)

where kG and kN are growth and nucleation rate constants,

respectively; C, solution concentration; Csat , saturated solution
concentration and Mc , solids concentration, and , volume and
surface shape factors, respectively, and c is the crystal density.
The value of the mass concentration exponent in secondary
nucleation kinetic (c) of Mc can be chosen based on the model
concepts: c = 0 for primary nucleation and the surface layer
mechanism in secondary nucleation, c = 1 for predominant interactions between the crystal and crystallizer or between the
crystal and the stirrer, and c = 2 for predominant crystalcrystal
interactions [20].
Table 2 presents the nucleation and final temperatures,
maximum undercooling temperatures and crystallization time
obtained in each experiment. As it can be observed, all the
processes were carried out with short times of crystallization
(900.016440.0 s).

E.A. Martnez et al. / Chemical Engineering and Processing 47 (2008) 21572162

2159

Table 2
Nucleation and final temperatures, maximum sub-cooling degree and time of
crystallization reached in each model experiment
Test

Tnucl ( C)

Tfinal ( C)

T ( C) = Tsat Tnucl

tc (s)

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27

24.30
26.27
25.67
16.82
20.50
22.43
16.91
14.96
16.76
38.81
38.38
38.89
29.90
33.52
35.14
29.88
30.39
31.02
51.54
48.58
50.03
50.78
48.18
49.19
48.65
46.20
45.44

5.88
6.23
5.81
6.30
6.17
6.18
7.22
7.27
7.26
15.89
15.81
15.75
16.55
16.23
16.25
17.34
17.08
17.09
24.94
24.79
25.93
24.85
24.88
24.84
27.06
27.88
26.99

15.70
13.73
14.33
23.18
19.50
17.57
23.10
25.04
23.24
11.19
11.62
11.11
20.10
16.48
14.86
20.12
19.61
18.98
8.46
11.42
9.97
9.22
11.82
10.81
11.35
13.80
14.56

11052.00
12025.80
11912.40
2525.40
3441.00
3900.60
1162.80
924.00
1139.40
13752.00
13541.40
13882.80
3205.20
4149.60
4533.60
1505.40
1596.00
1679.40
15958.80
16434.00
14456.40
6223.20
5594.40
5844.00
2591.40
2199.00
2214.00

In order to obtain the kinetics parameters by the Nyvlts

method, each data set of the CSD of the crystalline product
[M(L)] was converted into the adimensional z according to the
gamma function. This is the equation describing the dependence
of the oversize fraction on the crystal size:


z3
M(L) = 100 1 + z + z2 /2 +
exp(z)
6

(3)

where z [z = Lm /Gtc ] is a dimensionless crystal size; G is the

crystal growth rate; tc is the crystallization time and Lm is the
crystal mean size.
In this distribution the dependence of M(L) on the dimensionless crystal size (z) is marked by an inflection point
corresponding to the maximum value on the differential size
distribution where z = 3. The substitution of this value into Eq.
(3) yields the oversize fraction M(L) of 64.7% [16]. The values
of mean size (Lm ) were then determined from the linear relation
of z and L for z = 3 corresponding to the maximum value of M(L)
for each experiment.
Fig. 1 shows the differential distribution of the crystal sizes
for the experiments 22 and 24 carried out at 60 C saturation
temperature and 0.25 C/min cooling rate. As can be observed,
the measurements for each run showed a good reproducibility
since Lm values of 0.000429 m and 0.000430 m were obtained
for experiments 22 and 24, respectively. The values of L higher
than 0.001 m represented a smaller accumulated fraction and no
crystal with more than 0.002 m was produced.

Fig. 1. Differential distribution (M(L)) of the crystal sizes obtained in the experiments 22 and 24 carried out at 60 C saturation temperature and 0.25 C/min
cooling rate.

The increase in the cooling rate from 0.10 to 0.50 C/min, led
to a higher supersaturation state, and decreased the nucleation
temperature in 9, 8 and 3 C. On the other hand, the maximum
grade of solution undercooling increased in 9, 7 and 3 C for saturation temperatures of 40, 50 and 60 C, respectively (Table 2)
when the cooling rate was increased. The cooling rate used in
the crystallization process expresses the supersaturation magnitude, that is, lower values of cooling rate guarantee to work with
a lower supersaturation degree, which induces to lower values
of growth and nucleation rates.
The mean crystal size in the batch crystallizer product is
defined as [20]:
Lm = 3Gtc

(4)

and the average crystal growth rate (G) was then determined by
dividing the mean size by three times the crystallization time.
The suspension concentration can be calculated as:
 
6

4
(5)
c nN L4m
Mc = 6c nN (Gtc ) =
81
where Mc is the xylitol mass/solvent volume (kg/m3solv ); is the
crystal volume shape factor and c is the crystal density (kg/m3 )

and the symbol nN designates the nuclei population density:



dN/dt

nN =
(6)
G
The substitution of Eqs. (1) and (5) into Eq. (2) yields a simple
relation for the nucleation rate (dN/dt in #/m3solv s):
dN
27GMc
=
dt
(2c L4m )

(7)

Table 3 presents the values of crystal mass by solvent volume (Mc ), the average growth (G) and nucleation (dN/dt) rates
obtained in the xylitol crystallization process in ethanolwater
solutions.
Hao et al. [22] in a study on effect of methanol content on
crystallization kinetics of xylitol in a batch operated crystallizer
reported that the methanol content had an apparent effect on
nucleation and growth rates of xylitol. These authors reported
lower values of growth rate (0.025 109 m/s) and higher
values of nucleation rate (0.019.7 109 #/m3 s) in the crystallization of xylitol in methanolwater system. In a general way,
nucleation and growth rates of xylitol increased with the increase

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E.A. Martnez et al. / Chemical Engineering and Processing 47 (2008) 21572162

Table 3
Crystallized mass of xylitol (Mc ), growth (G) and nucleation (dN/dt) rates in the
model experiments
Test

Mc (kg/m3solv )

G (m/s) (108 )

dN/dt (#/m3solv s) (107 )

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27

782.91
782.49
785.82
788.94
766.47
783.53
778.75
742.13
783.95
1359.13
1340.59
1261.07
1333.34
1366.12
1294.12
1380.09
1327.43
1243.07
2392.87
2133.00
2329.87
2346.37
2122.50
2383.87
2326.87
2383.87
2291.25

94.34
82.71
126.50
503.14
286.20
244.50
1134.60
1122.95
836.72
88.89
108.83
77.38
317.11
311.24
251.66
858.32
929.90
622.71
102.29
102.44
83.83
225.77
236.05
260.43
506.50
894.35
588.27

0.837
0.885
0.258
2.04
3.12
3.10
3.90
9.62
10.6
0.724
0.414
0.981
5.30
2.05
2.57
5.69
3.41
8.66
0.461
0.364
1.21
1.82
2.21
1.55
5.32
1.91
6.27

Fig. 2. Correlation between nucleation and growth rates on log basis.

Fig. 3. Maximum value of T as a function of the cooling rate with 40 (), 50

() and 60 C () saturation temperatures, respectively.

of supersaturation and decreased with the increase of methanol

content under the same supersaturation condition.
From the logarithmic form of Eq. (7) the c, g/n and BN values
can be estimated by the multilinear correlation function:


 


n
kN
dN
+ c log(Mc ) +
= log
log(G)
(8)
log
n/g
dt
g
k
G

where n is the order of nucleation kinetics and g the order of the

overall crystal growth kinetics.
Fig. 2 shows the better correlation between nucleation and
growth rates on log basis which was obtained when c = 0. The
angular coefficient of this linear equation represents the n/g
ratio (equal to 0.9995). The interception or regression constant
n/g
log(kn /kg ) = A was 14.88. The determination coefficient (R2 )
was 0.7297, which indicates that the model of nucleation rate is

suitable for the process, and explains 73% the total variation in
the response as a function of the apparent growth rate.
The exponents g and n were separated through the determination of the apparent order of nucleation rate [m = (3g + n + 4)/4],
which is the linear coefficient from the plot of cooling rate (CR)
and maximum undercooling (T in C) data on log basis (Fig. 3).
A small variation between the angular coefficients (0.34, 0.30
and 0.22) for each initial xylitol concentration (Tsat = 40, 50
and 60 C) was observed, thus the average value (1/0.29) was
utilized.
Table 4 summarizes the kinetics parameters orders of nucleation (n) and growth (g), mass concentration exponent in
secondary nucleation kinetic (c), system kinetic constant (BN
in (kg/kgsolv )g/n sg/n1 ), regression constant (A ), determination
coefficient (R2 ) and calculated and tabulated Student t values
(tscal and tstab , respectively) obtained by taking all experiments
into account (N = 27) and not counting the essay number 26

Table 4
Values of kinetics parameters: exponents n and g, c, system kinetic constant (BN ), regression constant (A ), determination coefficient (R2 ) and calculated and tabulated
Student t values (tscalc and tstab )
Test

c
0.09
0
1
0.07
0
1

g/n
1.079
1.073
0.76
0.994
1
0.992

n
2.30
2.31
nd
2.43
2.44
2.61

g
2.48
2.48
nd
2.44
2.44
2.38

A (#/m3solv s)
14.60
14.35
nd
14.71
14.88
12.50

R2

BN (kg/kgsolv )g/n sg/n1

0.6798
0.6781
nd
0.7305
0.7297
0.6778

1.64 1016

tscalc

tstab

7.29
2.479
2.26 1016
7.26
nd
nd
5.52 1018
8.16
2.485
Without 26
4.76 1018
8.05
(N = 26)
nd
2.41 1014

where nd, not determined; the calculated Student t value was determined using the equation tscalc = (R (N 2))/ (1 R2 ) (Rodrigues and Iemma [23]) and the
tabulated values (tstab ) with 26 and 25 degrees of freedom at 1% probability level, respectively from Box et al. [24].
All (N = 27)

E.A. Martnez et al. / Chemical Engineering and Processing 47 (2008) 21572162

2161

Acknowledgements
The financial support of FAPESP, Brazil is gratefully
acknowledged. Thanks to Danisco Sweeteners Ltda., Brazil, by
the xylitol used in this work and Mrs. Lilian Marton Robin for
revising this paper.
Appendix A. Nomenclature

A
Fig. 4. The relationship between calculated (Lcalc ) and experimental (Lexp ) crystal size.

R2

(N = 26). As can be seen, the

was higher (0.7297) when the
results of the experiment numbers 26 were not considered. This
indicates that the values of G and dN/dt obtained in this experiment are far away from the others under the same condition. The
calculated Students t values were always higher than the tabulated values with N 1 degrees of freedom at 1% probability
level.
After rearrangement of Eqs. (1), (2), (5) and (6), Eq. (9) is
obtained which determines the crystal mean size in the model
experiments using different saturation temperatures and cooling
rates [20]:
 t (1g/n)
c
L(1+3g/n)
= 3 BN Mc(1c)(g/n)
(9)
m
3
and the system kinetic constant BN can be described by:


n/g g/n
4.5kG
(4.5g/n kG )
=
BN =
c kN
(c kN )g/n

(10)

Fig. 4 depicts the relation between calculated and experimental crystal sizes of xylitol and the correlation is almost equitable
around the line. As can be verified, the fitting between experimental and calculated crystal sizes has 11.30% mean deviation.
The obtained hypothetic distribution permits the determination
of modeling parameters and the estimate of crystal mean size
from different initial experimental conditions.
4. Conclusions
The Nyvlts methodology coupled with model experiments
was used to determine the kinetic parameters of batch cooling
crystallization of xylitol in waterethanol (50:50% w/w) solutions. The obtained kinetic parameters were: the order of crystal
growth kinetics (g = 2.44), the order of nucleation kinetics
(n = 2.44), apparent order of nucleation kinetics (m = 3.44), and
BN , the system kinetic constant (BN = 4.76 1018 kg/kgsolv ).
These parameters made possible to calculate the mean crystal size and to compare it with experimental values. The
fitting between experimental and calculated crystal sizes has
11.30% mean deviation. The obtained hypothetic distribution
permits the determination of modeling parameters and the estimate of crystal mean size from different initial experimental
conditions.

B*
BN
c
C
Csat
CR
CSD
dN/dt
g
G
kG
kN
L
Lcal
Lm
m
Mc
M(L)
n

nN
N
R2
tc
tscalc
tstab
Tsat
T
z

n/g

regression constant equal to log(kn /kg ) in Eq. (8)

(#/m3solv s)
secondary nucleation rate (#/m3 s)
system kinetic constant (kg/kgsolv )g/n sg/n1
mass concentration exponent in secondary nucleation
kinetic
solution concentration (kg/kg)
saturated solution concentration (kg/kg)
cooling rate ( C/min)
crystal size distribution
nucleation rate (#/m3solv s)
order of overall crystal growth kinetics
crystal growth rate (m/s)
growth kinetic constant
nucleation kinetic constant
crystal size (m)
calculated crystal size (m)
crystal mean size (m)
apparent order of nucleation
xylitol mass/solvent volume (kg/m3solv )
differential size distribution
order of nucleation kinetic
nuclei population density
number of experiments
determination coefficient
crystallization time (s)
calculated Student t value
tabulated Student t value
saturation temperature ( C)
maximum undercooling ( C)
dimensionless crystal size

Greek letters

crystal volume shape factor

crystal surface shape factor

c
xylitol density (kg/m3 )
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