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Received 13 January 2000; accepted 30 May 2000
Abstract
Cylindrical gelatin gels were frozen at atmospheric pressure with dierent operating conditions (air-blast freezing at dierent air
temperatures and brine freezing). A method to calculate a local freezing rate was proposed to take into account the variation of
freezing rate as a function of the radius. A linear evolution of the local freezing rate according to the radius was observed whatever
the freezing process was. Frozen gels were freeze-dried and sliced perpendicularly to the heat ux. The ice crystal marks were
measured according to the radial position with image analysis software. Each radial distribution of ice crystal size was characterised
by the mean representative diameter. A linear regression permitted to link the ice crystal mean representative diameter to the radial
position. On addition, the variation in the mean diameter with the local freezing rate was tted by a power law. 2000 Elsevier
Science Ltd. All rights reserved.
Keywords: Freezing; Ice crystal size; Gelatin gel; Cylindrical geometry
1. Introduction
Freezing is an ecient preservation process because
of the transformation of liquid water into ice which reduces greatly microbial and enzymatic activities. But ice
crystals formed during freezing have a great inuence on
the quality of foodstus after thawing causing drip
losses, textural and colour modications (Fellows,
1988). The size of ice crystals in a frozen sample depends
on the number of nuclei formed during freezing. Ice
nucleation is mainly initiated during the rst-degree fall
below the initial freezing temperature. Thus, it is important to control the operating conditions during this
phase to obtain good nucleation. It is well known that a
fast freezing rate tends to form a ne ice structure which
causes less damage to the structure of the product while
a slow freezing rate leads to large ice crystals (Reid,
1993). Although the relation between ice structure and
freezing rate in food have been mostly qualitative (Bello,
Luft, & Pigott, 1992; Grujic, Retrovic, Pikula, &
Amidzic, 1993), some studies have quantitatively related
;
1
tc
Ta Tf N h 4k
wx
0260-8774/00/$ - see front matter 2000 Elsevier Science Ltd. All rights reserved.
PII: S 0 2 6 0 - 8 7 7 4 ( 0 0 ) 0 0 0 8 9 - 3
Ta Tf
;
qDH 1=h x=k
278
Notation
coecient (m2 s1 )
coecient
representative ice crystal diameter (m)
mean representative ice crystal diameter (m)
maximum vertical distance between the cumulative distribution function of two samples in the KolmogorovSmirnov test
mass diusivity of water (m2 s1 )
temperature gradient in the j zone (C m1 )
heat transfer coecient (W m2 K1 )
enthalpy (J kg1 )
dendritic spacing (m)
characteristic dimension in Plank equation (m)
constant in Plank equation
radius (m)
a
b
dp
dp
Dobs
D
Gj
H
H
L
M
N
R
r0
R
tc
T
Ta
Tf
U
W
x
Greeks
k
thermal conductivity of the frozen food (W m1 K1 )
q
density of frozen sample (kg m3 )
Subscripts
1
frozen zone
2
unfrozen zone
Table 1
Characterisation of mean crystal size (technique of observation, range of size) in relation with freezing rate for slab geometry
Product
Freezing rate
Observation
technique
Alloys
Beef
Relation with
freezing rate
Reference
4060
dp / RG2
Freeze-substitution
1045
dp / 1=RG2
5200
dp / Rb
5500
L dp / 1=RG1 0:5
50500
dp / D=R
Sucrose
solutions
Apple tissue
0.031C/min450C/min
Protein gels
0.0030.02 m/h
Cryo-scanning
electron microscopy
Cryo-scanning
electron microscopy
Freeze-xation
Gelatin gels
Freeze-drying
10100
L dp / 1=RG1 0:5
Gelatin gels
with salt
Freeze-drying
50700
L dp / 1=RG1 0:5
wr
1.25C/min100C/min
Mean size
observed (lm)
Ta Tf
;
qDH r=r0 h r=kLnr0 =r
Innite slab
Innite cylinder
Thickness
Diameter
2
4
279
280
Fig. 1. Experimental cylindrical gel: size, thermocouples locations and presentation of the method to calculate the local freezing rate.
281
Fig. 2. Temperature proles during air-blast freezing with an air temperature of )20C and an air speed of 4 m s1 . Arrows indicate the radial
locations (mm) of thermocouples.
Fig. 3. Local freezing rate according to the radial position in a cylindrical 2% gelatin gel for air-blast freezing )20C (}), air-blast freezing
)30C (h) and brine freezing )20C (D).
282
and brine freezing at )20C processes are presented respectively in Figs. 5 and 6. Whatever the freezing
method was, the distribution was more and more dispersed with increasing radius. The relative cumulative
distributions of ice crystal size showed a decrease in the
size of ice crystal from the surface to the centre except
for the radius 18 mm. In the case of air-blast freezing
()20C and )30C), the relative cumulative distribution
of the surface (radius 18 mm) was smaller than the one
of the radius 14 mm. In the case of brine freezing
()20C), this relative cumulative distribution at radius
18 mm was smaller than those of the two next radii
(14 mm and 10 mm). This was probably due to the high
heat exchange between the cooling medium (air or brine)
and the surface of the sample at the beginning of freezing. For brine freezing this phenomenon is correlated
with the particular evolution of the local freezing rate at
the surface of the sample previously described. The
spread of ice crystal size with radius was much larger for
the air-blast freezing processes than for brine freezing.
A statistical analysis was carried out based on the two
samples KolmogorovSmirnov test to identify dierences between the dierent distributions in the same
sample. Results for each test are quoted for air-blast
Fig. 4. Sections of freeze-dried cylindrical 2% gelatin gel frozen by airblast with a cooling temperature of )30C: (a) sliced parallel to the
heat ux ( 6.4); (b) sliced perpendicular to the heat ux ( 80).
283
Table 5
Pairwise comparisons of brine freezing ()20C) radial distributions by
KolmogorovSmirnov tests. In each cell, the rst value is Dobs and the
second one (bold character) is the P-value
Radius (mm)
14 mm
10 mm
6 mm
2 mm
Radius (mm)
14 mm
10 mm
4 mm
2 mm
18
0.24
(<0.00)
0.15
(0.014)
0.37
(<0.00)
0.35
(<0.00)
0.69
(<0.00)
0.16
(<0.00)
0.61
(<0.00)
0.78
(<0.00)
0.43
(<0.00)
0.30
(<0.00)
18
0.13
(0.02)
0.10
(0.21)
0.11
(0.17)
0.21
(<0.00)
0.27
(<0.00)
0.28
(<0.00)
0.24
(<0.00)
0.34
(<0.00)
0.34
(<0.00)
0.09
(0.26)
14
10
6
Table 4
Pairwise comparisons of air-blast freezing ()30C) radial distributions
by KolmogorovSmirnov tests. In each cell, the rst value is Dobs and
the second one (bold character) is the P-value
Radius (mm)
14 mm
10 mm
6 mm
2 mm
18
0.34
(<0.00)
0.40
(<0.00)
0.32
(<0.00)
0.69
(<0.00)
0.60
(<0.00)
0.33
(<0.00)
0.83
(<0.00)
0.69
(<0.00)
0.43
(<0.00)
0.17
(0.03)
14
10
6
14
10
4
284
A local freezing rate has been dened to take into account the change in freezing rate according to the radial
location. This local freezing rate changes inversely to the
representative diameter as a function of the radius.
These conclusions are very dierent from those obtained
with unidirectional heat ow freezing obtained in a slab.
Acknowledgements
4. Conclusion
As a conclusion the freezing of cylindrical gelatin gels
cooled on each face showed a decrease of the ice crystal
size with the increase in distance to the cooling medium.
Thanks to the French Ministry of Agriculture for nancial support (Ph. D. grant) and to Region Pays de
Loire and P^
ole Agronomique Ouest for supporting the
experimental cost. Thanks to Dr. H. S. Ramaswamy for
help in preparing the manuscript. Thanks to P. Cantoni
for technical support for image analysis.
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