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Fundamental
Principles of Ultrafiltration
ANN-SOFI
J6NSSON*
Department
GUNTRAGARDH
Department
(Received
Abstract
Different theoretical models describing the influence of the operating parameters are treated in this paper. The
osmotic pressure, gel layer and resistance in series models are presented. The influence of different operating
parameters, such as the operating pressure, temperature, cross-flow velocity and concentration is demonstrated.
The complex fouling phenomenon is reviewed. Finally, various pretreatment and cleaning operations are
presented.
Introduction
Ultrafiltration
(UF) has become an important
industrial operation in many areas of application. A
highly successful application of ultrafiltration is the
recovery of electrodeposition
paints [ 1, 21. This
application is so established that ultrafiltration
equipment is considered a standard part of all electrodeposition systems nowadays.
A large number of commercial ultrafiltration
plants are also in operation in the food industry
[3-61. The separation of oil-water emulsions [7] and
the treatment of industrial effluents from the pulp
and paper industry [8] are other important applications.
Although commercially successful in many areas,
the complex, fundamental mechanisms of the ultrafiltration process are still poorly understood.
Ultrafiltration of macrosolutes causes an instantaneous and inevitable reduction in flux relative to the
pure water flux of the membrane. The polarization
phenomenon to which this loss of flux is attributed
has been explained by classical fluid mechanical and
mass transfer theory. The three most widespread
theories are
- the osmotic pressure model,
_ the gel layer model, and
- the resistance in series model.
As a result of fouling there is also a flux decline
which is not reversible by simply altering the operating conditions. Thus, the problem of fouling is often
superimposed upon the concentration polarization.
Its severity depends on the membrane material, the
*To whom correspondence should be addressed.
02552701/90/%3.50
27 (1990) 67-81
68
the membrane.
For example, a membrane
that is
cleaned before use has quite a different performance
than that of one that has not been cleaned.
Real-life
performance
Influence
of pressure
de-
KAP
p AL
(1)
where J is the water flux, K is the specific permeability of the medium, AP is the pressure difference
across the medium, p is the fluid viscosity and AL is
the thickness of the medium.
It is, however, difficult to measure the effective
thickness of an asymmetric membrane. The thickness
and the specific permeability
of the membrane are
therefore usually combined to form a medium-specific parameter, the hydraulic resistance of the membrane, R, = AL/K.
In ultrafiltration,
solutes and/or particles are retained by the porous medium, the membrane.
This
makes the introduction
of more involved relations
than eqn. (1) necessary.
Solute is transmitted
by convection
towards the
membrane
as soon as the transport
of solvent
through the membrane commences, and the concentration is increased on the feed side of the membrane
as solute is retained. The osmotic pressure difference
Ail across the membrane can then become substantial. The driving force of the fluid is in this case given
by AP - c AD, according
to the three-parameter
model of Kedem and Katchalsky
[ 10, 111. The reflection coefficient 0 indicates the degree of permselectivity of the membrane. When CJ = 1 the solute is totally
retained and when 0 = 0 it is totally permeable.
The resistance of the accumulated
solute at the
membrane
surface is sometimes
represented
as a
hydraulic resistance R,. If we introduce hydraulic
resistances instead of permeability in Darcys equation and take the osmotic pressure of the solute into
consideration,
the ultrafiltration
flux
scribed by the generalized equation
may
be de-
AP--AII
J=
/4%+%)
models
pressure
model
69
where c,, is the concentration in the permeate and k
is the mass transfer coefficient.
Taking the osmotic pressure at the membrane
wall into account, Wijmans et al. [ 131 have derived a
relation between pressure and flux. Their calculated
results have been found to be in good accordance
with experimental results [ 141.
Wijmans et al. [ 131 used the following relationship
between the osmotic pressure and the concentration
at the membrane wall:
I
(4)
lT, = ac,
(5)
11&
= = l/(pR,)
(6)
250
f
200
150
100
50
0
0.2
0.4
0.6
PRESSURE
0.8
1.0
1.2
(MPa)
Fig. 2. The effect of operating pressure on flux for three ultrafiltration membranes with varying permeabilities, calculated using
eqn. (5). The PWPs of the three membranes were 1000, 250 and
1C01m-2h-
MPa-
at
T=2OC
(this
corresponds
to
& = 3.6 X 102, 14.4 x 10 and 36.0 x 10tZm~, respectively).
Lines without symbols represent the pure water fluxes of the three
membranes and lines with symbols represent the flux of a
1.0 wt.% solution (c, = O.Ol), which has an osmotic pressure of
0.1 MPa at a concentration of 10 wt.% (a = 10 MPa and n = 2).
This applies fairly well to solutions of dextran [ 141. The value of
the mass transfer coefficient was 2 x 10m5 m SK.
dJ=L(l
d AP
pR,
+A!%)-
2
(8)
0
In the gel layer model the osmotic pressure is
assumed to be zero. The fluid flow is then described
by
AP
J=
(9)
14Rm + Rs)
When the concentration
at the wall has not
yet reached the gel concentration,
the polarized
70
boundary layer offers a resistance to the flux,H&,
and R, = R,, . Under gel layer conditions
the resistance of the gel layer represents the resistance of the
solute, R, = R,. When both concentration
and gel
polarization
occur the resistance
of the solute is
R,= R,+Rb,
[15].
The gel layer model predicts the flux to be independent of operating pressure. An increased pressure
merely results in a thicker gel layer (larger &),
which retards the flux to its original value.
The gel layer model has been frequently used to
correlate experimental
limiting fluxes [ 16- 181. The
gel concentration
may be obtained by extrapolation
of a plot of J versus In cb. It has, however, been
shown that the information
obtained on gel concentrations is not reliable. For identical solutions different authors have found widely varying values at cg
[191.
Experimental
evidence [ 151 indicates that the viscous solution in the boundary layer approaches
a
close-packed
configuration
of low hydraulic permeability. It has been argued, however, that it is only
materials
such as agar, pectin, gelatin and some
proteins that might denaturate
at the membrane
surface to give true gels [ 141. It has also been shown
that feed solutions
of various macrosolutes
with
concentration
cb = cg did not give zero flux [20].
Based on their analysis, Wijmans et al. [ 131 concluded that osmotic pressure limitations would be
expected in the ultrafiltration
of macrosolutes
with
molecular weights of 10 000- 100 000, and gel layer
limitations would be expected for larger molecules.
The resistance in series model
The concentrated
solution of macromolecules
at
the membrane
wall provides a physical barrier to
solvent and solute transport. The resistance of this
boundary
layer may be treated as one or several
resistances in series with the membrane,
as already
discussed in the gel layer model.
The resistance in series model has been shown to
apply for dextran solutions [21]. The resistance of
the solute in this investigation
was estimated from
independently
measured sedimentation
coefficients.
The results were also in reasonable agreement with
results obtained from the osmotic pressure model.
The resistance in series model predicts a pressureindependent flux, as does the gel layer model. That is
to say, an increase in the pressure results in a thicker
gel layer and an increased hydraulic resistance.
An advantage with the resistance in series model
is that it makes it possible to distinguish between th0
influence of different flux decline phenomena.
The resistance to flow may be accounted for by a
number of resistances: the resistance R, of the membrane, the boundary
layer resistance
R,,, the gel
layer resistance R,, and the adsorbed layer resistance
R,. Equation (2) may then be written as
AP
J=p(R,+R,+R,+Rh,)
(10)
01
1000
2000
ROTATION
3000
SPEED
b
4000
(rpm)
Fig. 3. Determination
of the influence of the membrane
resistance, boundary layer resistance, gel layer resistance and adsorbed
layer resistance
for 1.0 wt.% BSA at 0.5 MPa. The numbers
denote the order in which the measurements
were performed. The
rotary module is described in detail in ref. 22.
(11)
71
ciable extent by the low applied pressures that are
encountered during ultrafiltration. It is, however, a
reasonable assumption that as the porosity of the
membranes increases, the susceptibility to deformation also increases.
For a membrane with surface porosity S,, and
cylindrical membrane pores with radius rp, the
Hagen-Poiseuille
equation [ 241 applies:
S, rp2 AP
8pAL
J=
(12)
(13)
rZ12
where A, is a proportionality constant and AL is the
membrane thickness. Equation ( 13) shows that even
a modest decrease in the pore radius may lead to a
significant increase in the resistance of the membrane.
The hydraulic permeability of a gel, Kg, may be
approximated by the Kozeny -Carman relation [ 151,
R,=-
(4 &I2
180(1 -E)~
(14)
(1%
is thus obviously very sensitive to the molecule size
and porosity. AL, in eqn. (15) is the thickness of the
gel layer.
The porosity of the gel, E, and the pore size of the
membrane, rp, are affected by the operating pressure.
The porosity of the gel, as well as the membrane
pore radius, decreases (at least to some extent) when
the pressure increases. This results in increasing hydraulic resistances, according to eqns. ( 13) and ( 15).
The increasing hydraulic resistances would then explain why flux may decrease when the operating
pressure is increased.
Furthermore, for many porous materials compression is an irreversible process. When the pressure
is decreased the material does not expand to its
original size. This means that if a high pressure has
been applied to the gel layer, the flux may not be
restored by decreasing the pressure again.
Influence
of temperature
250,
0.2
0.4
0.6
PRESSURE
0.8
1.0
1.2
(MPa)
Fig. 5. The influence of pressure on pure water Aux and ultrafiltration flux at 20 and 60 C. The values of the parameters in eqn.
(5)were:PWP=2501m-Zh-MPa-at
T=20C(R,=1.4x
IO m-l),
AP = 0.5 MPa, cb = 1.0 wt.%, k = 2 x 10e5 m SK,
n=lOMPaandn=2.
sideration, predicts, however, a less pronounced dependence. The deviation from the ideal behaviour
(the pure water flux) increases when the conccntration increases, as can be seen in Fig. 4.
The difference between the idea1 behaviour and
the real flux becomes larger as the temperature is
increased. This is quite natural as the concentration
polarization, and thus the osmotic pressure at the
membrane, increases when flux increases as a consequence of the elevated temperature. This phenomenon is also illustrated in Fig. 5.
The membrane resistance R, is not influenced by
variations in the temperature, whereas the pure water flux is. This means that when studying the influence of pressure at different temperatures a new
PWP line is obtained at each temperature. As can be
seen in Fig. 5 the difference between the pure water
and ultrafiltration flux becomes larger as the temperature and pure water flux increase. This is in analogy
with the behaviour shown in Fig. 2, where we
demonstrated that the difference between the pure
water and ultrafiltration flux was largest for the
membrane with the highest PWP.
Influence of feed concentration
A general trend is that flux decreases as the bulk
concentration increases (see point (4) under General
72
250
200
200
150
150
100
100
50
50
0
0
10
CONCENTRATION
Fig.
ing
eon.
(R,
n =
15
20
IN BULK (w-%)
trends). The film model (eqn. (3)) predicts, for example, that the flux J varies proportionally with the
logarithm of the bulk concentration ct,, and the gel
layer model predicts that the intercept of a plot of J
versus In ct, corresponds to the gel concentration cg.
The variation of flux with concentration, as predicted by the osmotic pressure model (eqn. (S)), is
shown in Fig. 6.
The flux is, as expected, higher at the high operating pressure. But, although the pure water flux (at
c,, = 0 in Fig. 6) is doubled when the pressure is
doubled, this considerable difference between the two
flux curves vanishes as the concentration increases.
The two flux curves in Fig. 6 approach zero at the
bulk concentration at which the osmotic pressure
equals the operating pressure. It is thus possible to
increase the final concentration of the solution by
increasing the operating pressure.
The osmotic-pressure-concentration
relationship
of the solution not only determines the final retentate
CONCENTRATION
two
and
and
eqn.
and
d In ct,
150
IN BULK (W-/o)
1 + &, k/AII n
(16)
125
100
E2
=
s
k
The mass
75
trader
coefficient
50
25
CONCENTRATION
IN BULK
(W-%)
where d,, is the hydraulic diameter of the flow channel, D the diffusivity, and Sh, Re and Sc are the
Sherwood, Reynolds and Schmidt numbers. The
constants A, a, b and c vary with flow conditions.
The mass transfer coefficient has been shown to
have a slight tendency to decrease with increasing
pressure and bulk concentration [ 121. The decrease
in flux with increasing pressure at elevated pressures
73
was suggested earlier in this paper to be the result of
the compaction of the membrane and gel layer at
high pressures. The decrease in the mass transfer
coefficient with increasing pressure has been put
forward as another explanation of this phenomenon
[141.
The diffusivity of macrosolutes is usually dependent on concentration. Owing to the concentration
polarization, the concentration at the membrane surface may differ significantly from the concentration
in the bulk, This may, of course, modify the effective
mass transfer coefficient. The diffusivity is also increased by an increase in the temperature. However,
the operational parameter that has the largest impact
on the mass transfer coefficient is the cross-flow
velocity.
Influence
of the cross$ow
velocity
(m/s)
two
and
and
(5)
at
01
10
(m/s)
modules
The ultrafiltration flux of a membrane is controlled by the rate at which the retained solutes can
be transferred from the membrane wall back into the
bulk fluid. Thus, operational variables that aid backtransport from the membrane will directly increase
the flux.
The shear rate at the membrane wall is, as has
been clear from the above, the major depolarizing
parameter. This fact initiated the development of
rotating modules [26,27]. However, the commercial
success of rotating modules has been limited (due to
high investment costs).
Positive results from tests with a modified plate
and frame rotary module, the ABB CROT filter,
have been reported recently. In pilot-plant equipment, bleaching effluent from a Swedish pulp mill
has been treated successfully over a one-year period.
A larger pilot plant (membrane area 200 m2) has
recently been installed at the same mill.
During ultrafiltration of oil emulsions in a rotary
module it was found that the flux could be increased
further if the roughness of the module wall was
increased [28]. The increase in the wall roughness
was accomplished by the introduction of a net. The
increase in the flux was ascribed to an increase in the
mass transfer coefficient due to the presence of the
net, acting as a static convection promoter.
74
It has also been shown that the mass transfer
coefficient can be increased, not only by increasing
the wall roughness, but also by using corrugated
membranes [29]. It was found that corrugations increased the mass transfer more effectively than an
increase in the cross-flow velocity. These tests were,
however, performed with reverse osmosis membranes, but a similar type of effect of membrane
surface roughness has been demonstrated for ultrafiltration membranes [ 301.
Influence
of suspended
(a)
:,:,:>
D
\\I
\\\
,.;<;.;
(b) ...
solids
Walk.
of time
(18)
many exceptions to the general rules reflect the complexity of the fouling phenomenon. (One sometimes
has the feeling that there are more exceptions than
rules.) Comprehensive information may, however, be
found in a number of review articles treating this
subject (see, for example, refs. 31 and 38-41).
The fouling process has variously been ascribed to
the formation of a slowly consolidating gel layer and
to membrane pore plugging. The former event may
occur if the solute molecules are large enough to be
retained by the membrane. This is illustrated in Fig.
1 l(a). As the gel layer is consolidated the hydraulic
resistance Rg increases continuously with time.
If, on the other hand, the solute molecules are
small enough to enter the pores they may be adsorbed
onto the pore walls, as can be seen in Fig. 1 i(b). The
adsorbed molecules can then restrict the effective pore
diameter and the membrane resistance R,,, increases
as a consequence of the pore blocking.
Retention
characteristics
Characteristic
pore sizes were determined
for
clean and fouled membranes
by Hanemaaijer
et al.
[45]. The pore size changes caused by solute adsorption were derived from saccharide retention data. It
was shown that for a hydrophilic
low protein adsorbing membrane,
the calculated pore size was not
affected by protein adsorption,
whereas the pore size
of hydrophobic
membranes
was reduced.
Adsorption
of one of the solutes in a mixture may
thus also affect the retention
of other compounds.
Solutes that are not retained by the membrane when
tested alone may very well be retained due to solutemembrane
and solute-solute
interactions
of other
compounds
in the solution.
It is thus advisable to
confirm the expected retention
characteristics
of a
membrane by tests with real solutions and not base
predictions
of membrane performance
on tests with
idealized solutions.
But even predictions
based on
tests with real solutions
may be unreliable
as the
composition
of many process streams may occasionally differ.
Influence
of membrane
material
It is commonly
recognized
that hydrophobic
membranes
have a larger fouling tendency than hydrophilic membranes.
Even the pure water flux may
be affected by the nature of the membrane material
as absolutely
pure water is very hard to find (a
well-known
problem
for anyone who works with
membranes).
Investigations
[ 3 1,46,47]
have shown that the
pure water flux of hydrophobic
membranes decreases
with time, while the pure water flux of hydrophilic
membranes is less time dependent. This phenomenon
has been attributed
to contamination
of the pure
water by bacteria and trace colloids [31] and to trace
amounts of waste products of micro-organisms
[46]
present in the pure water.
Infruence
of membrane
pore size
Membrane
performance
cannot, however, be related simply to the membrane material. For example,
the flux decline of three membranes,
all made of
polysulphone,
was noticeably different when the pH
of a BSA solution was altered [48].
The same disparate behaviour was found for three
membranes
with varying pore sizes used for the
treatment
of caustic bleach plant effluent [49]. The
effect on the flux of the three membranes
when the
pH was lowered differed considerably,
as can be seen
in Fig. 12.
At the higher pH the flux of all three membranes
was almost identical, while when the pH was lowered
to below the isoelectric
pH of the solution,
the
magnitude
of the flux followed the cut-off of the
membranes,
that is, the densest membrane
experienced the largest flux decline, while the flux of the
membrane with the largest pores was unchanged.
It was thus the membrane with the smallest pores
that exhibited the greatest flux decline in this case.
-0
20
40
80
100
TIME (h)
(a)
200
150
zj
100
ii
50
0
20
40
80
100
TIME (:;
(b)
of surfactants
76
surfactant solutions, for example, the membrane material, the pore size of the membrane and, of course,
the nature of the surfactant.
Surfactants
concentration
600
506
406
300
266
160
100
200
300
400
500
TIME (h)
Fig. 13. Variation of flux during addition of the non-ionic surfactant Triton X-100. The polysulphone membrane, DDS GRIO, has
a nominal cut-off of 500 000. The line with the open circles shows
the Aux decline of a membrane that has only been conditioned
with pure water. The line with the solid dots shows the flux decline
of the same membrane, but after cleaning of the membrane with
a commercial alkaline cleaning agent, Ultrasil 10 from Henkel.
Surfactant was added stepwise, the concentration 0.1 CMC, for
example, indicates that the concentration was 10% of the critical
micelle concentration. The operating pressure was 0.1 MPa and
the temperature 30 C.
hydrophobic tall
(b)
Fig. 14. (a) A charged solute is repelled by a membrane of the
same charge. (b) At the isoelectric pH the solute is uncharged and
may be adsorbed onto the membrane.
77
During ultrafiltration of kraft black liquor it was
found that large molecules, that were able to permeate the membrane at a high ionic strength, were
almost completely retained at low ionic strength [60].
The influence of pH may be altered if salt is
present in the solution. This has been demonstrated
for BSA [LX]. In the absence of salt the flux was at its
minimum at the isoelectric pH. In the presence of
0.2 M NaCl the flux was lowest at pH 2 and increased monotonically with increasing pH.
The zeta potential
of the membrane
t(351.
Centrifugation is often used, for instance to remove fines from whey and fibres from starch processing waters. Another example is centrifugation of
usually trial and error investigations, whereas systematic studies are very rare. Temperature, time,
concentration and type of surface active agent are
important cleaning parameters that vary with foulants and membrane material.
As a rule, mineral deposits are removed by acids
and proteins by alkaline solutions. For some products, it is necessary to use different chemicals in
succession to obtain a satisfactory cleaning result.
For milk, where protein deposits dominate, an alkaline formulation is used first, sometimes followed by
acid treatment to remove mineral deposits. If polysulphone membranes are used, a final alkaline cleaning is often carried out in order to improve the flux.
For whey, where mineral deposits dominate, acid
cleaning is often performed first, and is then followed by alkaline cleaning.
Some care is recommended when selecting a
cleaning procedure since an injudicious choice could
be catastrophic. As an example, in ref. 67 it is shown
that pectine, present in fruit juices, presents difficult
fouling problems. Especially alkaline detergents, and
also unsuitable acid products, may lead to complete
clogging of the membranes.
In order to obtain a good mechanical cleaning
effect, the cross-flow rate is often higher and the
pressure lower during cleaning than during normal
operating conditions.
Cleaning solutions are often a mixture of chemicals. Alkaline cleaning solutions usually contain
sodium hydroxide, phosphate, sequestering agents
and surface active agents. Examples of some cleaning
chemicals and the concentrations used are given in
Table 1.
The choice of surface active agent is very important, since some types may be adsorbed onto the
membrane surface, resulting in a flux reduction. On
the other hand, with a suitable choice of surfactant
in the cleaning solution considerably enhanced fluxes
may be obtained. Thus, as stated previously, it has
been suggested [49] that cleaning may be considered
not merely as a cleaning operation, but also as an in
situ surface modification.
The influence of the surfactant on the flux was
demonstrated in an investigation where membranes
fouled during ultrafiltration of whey were cleaned
with different types of surfactants [68]. Considerably
improved whey fluxes were experienced after cleaning with a solution containing an anionic surfactant,
TABLE
I. Examples of concentrations
cleaning and disinfection solutions
Cleaning/disinfecting
Caustic soda
EDTA-Na,
Nitric acid
Chlorine
Hydrogen peroxide
Sodium bisulphite
agent
of chemicals
Concentration
0.5-1.0
0.5-1.0
0.3-0.5
0.002-0.02
0.1
0.25
used in
cleaning
(%)
Concluding remarks
Our understanding of the fundamental principles
of ultrafiltration is becoming better and better. But
there is still a long way to go before the complex
mechanisms of the ultrafiltration process are fully
79
understood. A vast number of empirical investigations show that it is very hazardous to make general
statements, especially about the influence of different
parameters on fouling.
Experience indicates that if we are to be able
to describe the dynamics of ultrafiltration it will
be necessary to combine knowledge from different
areas. The theoretical models must combine knowledge and experience of fluid mechanics, mass transfer and surface chemistry phenomena.
Nomenclature
A*
A
a
a
b
c
cb
57
CP
:
4
4
J
JO
K
Kg
KO
k
L
AL
AL,
AP
PWF
PWP
n
n
R
&I
4
&
RS
Re
rP
SP
SC
Sh
t
u
0:
&
L-I
mv
d
Refereoces
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2 B. R. Breslau, A. J. Testa, B. A. Milnes and G. Medjanis,
Hollow fiber ultrafihration technology,Iti. WurerEng., 17
(1980) 20-26.
3 I. H. Hanemaaijer, Toepassing van membranfdtratie in de
zuivelindustrie, Voedingsmiddelen Technol., I8 (4) (1985) 2629.
4 V. Gekas, B. Hallstrom and G. Tr&$rdh, Food and dairy
applications: the state of the art, Desalinufion, 53 (1985)
95-127.
5 J.-L. Maubois, Recent developments of ultra8ltration in dairy
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and Membrane Processes, Plenum Press, New York, 1986, pp.
255-262.
6 R. M. Hedges and P. Pepper, Reverse osmosis and ultraliltration-advances
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Netherhzndv, Int. Fed. Fruit Juice Producers, 1986, pp. 253260.
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Desalination,
51
(1984) 61-77.
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of uhrafiltration membranes:
the osmotic pressure model, in G. Trlg&rdh (ed.), Proc. Conf.
on Characterization
of Ultrafiltration
Membranes,
&en&
Sforr, Sweden, Studentlitteratur, Lund, 1988, pp. 125- 140.
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(ed.), Membrane Science and Technology, Plenum Press, New
York, 1970, pp. 47-97.
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234-248.
17 A. G. Fane, C. J. D. Fell and A. G. Waters, The relationship between membrane surface pore characteristics and flux
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18 M. W. Chudacek and A. G. Fane, The dynamics of polarisation in unstirred and stirred ultrafiltration, J. Membr. Sci., 22
(1984) 145-160.
19 P. De.jmek, Concentration
polarization
in ultrafiltration of
macromolecules, Ph.D. Thesis, Dept. Food Engineering, Lund
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