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Journal of Food Engineering: Jir Í Blahovec, Stavros Yanniotis
Journal of Food Engineering: Jir Í Blahovec, Stavros Yanniotis
Journal of Food Engineering: Jir Í Blahovec, Stavros Yanniotis
a r t i c l e i n f o a b s t r a c t
Article history: A new equation is developed in this paper which is further used to divide sorption isotherms into classes
Received 20 December 2007 which are connected to surface water effects and/or solution water effects and their combinations. It is
Received in revised form 11 August 2008 shown that sorption isotherms can be successfully classified using the new equation into three basic clas-
Accepted 11 August 2008
ses I, II (most frequent) and III which roughly correspond to the original Brunauer’s classes. The equation
Available online 19 August 2008
is also used for further division of class II into three subclasses. Criteria for these classifications are
presented.
Keywords:
Ó 2008 Elsevier Ltd. All rights reserved.
Sorption
Isotherm
GAB
HH equation
Food
Polynomial
Water
Activity
Classification
1. Introduction logical origin. The GAB isotherm has been particularly successful
for water activities up to 0.9 (van den Berg, 1984).
Sorption isotherms represent the relation between water con- Brunauer classified sorption isotherms according to their
tent and water activity of any material at a given temperature. shape and processes which controlled the shape (Brunauer,
The water activity is then defined as the ratio of the water vapour 1943). Brunauer’s classification (I) represents Langmuir and/or
pressure above the material to the vapour pressure of pure water similar isotherms which show a characteristic increase in water
at the same temperature. The sorption isotherms provide impor- activity with increasing moisture content, and the first derivative
tant information on the product stability in relation to microbial of this plot increases with the moisture water content. This type
and enzyme activity (Karel, 1975). This is why the sorption iso- of sorption isotherm is typically applicable for filling the water
therms of foods and agricultural products have been extensively monomolecular layer at the internal surface of a material. The
studied; the list of the measured isotherms even at the beginning sigmoidal sorption isotherms, like BET and/or GAB equations,
of 1980s numbered more than a thousand (Iglesias and Chirife, represent the type II of the Brunauer’s classification. This type
1982). takes into account the existence of multilayers at the internal
A large number of theoretical and empirical models have been surface of a material. The isotherms of type III (Brunauer’s clas-
used to describe sorption isotherms. Van den Berg and Bruin sification) are relatively rare (Adamson, 1976). They are charac-
(1981) classified the 77 most important models into three groups: terised by the moisture content increasing with water activity
theoretical (48), partially theoretical (15), and fully empirical (14). in such a manner that the first derivative of moisture content
The crucial equation among the theoretical models is the Lang- also increasing with increasing water activity. This type of sorp-
muir’s isotherm which is based on the forces acting between the tion isotherm is observed frequently in the case of solids soluble
product surface and the water condensed from the vapour as a in water e.g., sugars and it is described by formulae similar to
monomolecular layer. The extensions of the Langmuir’s underpin- Raoult’s Law. The more complicated sorption isotherms of IVth
ning idea to multi molecular layers result in the BET and GAB iso- and Vth classes of the Brunauer’s classification are frequently ob-
therms which are able to describe sigmoidal shape isotherms served in the case of capillary condensation (Adamson, 1976)
commonly observed in the case of food and other materials of bio- where sorption depends sensitively on the distribution of pore
dimensions.
* Corresponding author. Fax: +420 234381828. The class II isotherms in the GAB form can be interpreted as
E-mail address: blahovec@tf.czu.cz (J. Blahovec). a superposition of the localised monolayer adsorption on the
0260-8774/$ - see front matter Ó 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jfoodeng.2008.08.007
J. Blahovec, S. Yanniotis / Journal of Food Engineering 91 (2009) 72–77 73
internal material surface and the dilution of some part of the solids aw A aw AE
¼ þ B
in solution (van den Berg, 1984). The mathematical expressions for w D D D w
!" !#
this theory were developed originally for polymer hydration by
a2 EB AE2 X1 Eaw i
Hailwood and Horobin (1946). þ w C1 þ 2 ð2dÞ
In this paper, we develop a new equation which not only suc-
D D D i¼0 D
cessfully describes experimental sorption data but can also be used
as a basis for the classification of the sorption isotherms observed The quadratic term in Eq. (2d) is modified in the infinite sum that
in foods. can be summed as two infinite geometric series, obtaining the fol-
lowing equation
!
aw A aw AE a2 EB AE2 1
2. The proposed equation ¼ þ B w C1 þ 2 ð2eÞ
w D D D D D D 1 þ DE aw
The Langmuir isotherm is one of the best known adsorption
Eq. (2e) shows that the proposed Eq. (2) gives for aw/w a polynomial
models which apply up to monolayer coverage. It can be expressed
expression similar to the basic HH model does but with modified
in the following form (van den Berg and Bruin, 1981)
parameters. For the special case where E = 0, Eq. (2e) corresponds
wL C L aw to the ‘G.A.B.’ equation
¼ ð1Þ
wm 1 þ C L aw aw A B C1
¼ þ aw a2w ð2fÞ
where wL is the moisture content (d.b.); wm is the monolayer value; w D D D
aw is the water activity and; CL is a fitted parameter. where
Eq. (1) can be rewritten into the alternative form
A 1
aw ¼ ð3aÞ
wL ¼ ð1aÞ D wm KC
a1 þ b1 aw
where a1 ¼ ðC L wm Þ1 and b1 ¼ ðwm Þ1 . B 1
¼ ðC 2Þ ð3bÞ
For real solutions, water activity is given by D Cwm
wSR
aw ¼ cX w ¼ c ð1bÞ C1 K
wSR þ ns ¼ ðC 1Þ ð3cÞ
D Cwm
where c activity coefficient; wS = 18.02 wSR, the water content of
the solution; ns is the moles of the adsorbing solute in the solu- are related to the usual C, wm, and K, the ‘G.A.B.’ parameters used in
tion.Rearrangement of Eq. (1b) gives Eq. (2c).
Eq. (2e) can be simplified when new parameters X1, X2, X3, and
aw
wS ¼ ð1cÞ X4 are defined
a2 b2 aw
aw a2w
where a2 = c/(18.02 ns) and b2 = (18.02 ns)1. ¼ X 1 þ ðX 2 X 1 X 4 Þaw ðX 3 þ X 2 X 4 X 1 X 24 Þ ð4Þ
If we consider that the water in foods adsorbs in the form of a w 1 þ X 4 aw
localized monolayer on the internal material surface and dilutes where
some part of solids in a complex solution of salts, sugars and pro-
teins, the superposition of Eqs. (1a) and (1c) will give the total A a1 a2
X1 ¼ ¼ ð4aÞ
amount of water adsorbed in a food. Thus D a1 þ a2
aw aw
w¼ þ : ð2Þ B a2 b1 a1 b2
a1 þ b1 aw a2 b2 aw X2 ¼ ¼ ð4bÞ
D a1 þ a2
The first term in Eq. (2) represents the amount of water bonded to
the sorption sites of the solid and the second one represents water C1 b1 b2
X3 ¼ ¼ ð4cÞ
present in the complex aqueous solution of the food. When D a1 þ a2
b1 = b2 = b, Eq. (2) takes the form of the Hailwood and Horobin’s
(‘HH.’) sorption equation (Hailwood and Horobin, 1946) E b1 b2
X4 ¼ ¼ ð4dÞ
aw aw D a1 þ a2
w¼ þ : ð2aÞ
a1 þ baw a2 baw where ai and bi are parameters in Eq. (2).
Eq. (2a) can be rewritten into the ‘G.A.B.’ equation, in which a1 = Eq. (4) can be simplified now into the final form
1/[wm(C1)K], a2 = 1/[wmK], and b = 1/wm are related to the stan- aw a2w
dard ‘G.A.B’ variables wm, K and C (van den Berg, 1981) ¼ X 1 þ X 02 aw X 03 ð4eÞ
w 1 þ X 4 aw
wm CKaw using new parameters X 02 and X 03
w¼ : ð2bÞ
ð1 Kaw Þð1 Kaw þ CKaw Þ
X 02 ¼ X 2 X 1 X 4 ð4fÞ
For Eq. (2), the ratio aw/w is expressed as follows
aw A þ Baw C 1 a2w X 03 ¼ X 3 þ X 2 X 4 X 1 X 24 ¼ X 3 þ X 4 X 02 ð4gÞ
¼ ð2cÞ
w D þ Eaw
where A = a1a2, B = a2b1a1b2, C1 = b1b2, D = a1 + a2, E = b1b2. When 3. Properties of the proposed equation
E = 0, i.e., b1 = b2, Eq. (2c) gives the regular formula (van den Berg,
1981) that is used for approximation of sorption data by the Eq. (2d) has interesting properties predetermined by the
‘G.A.B.’ equation. Eq. (2c) can be expressed by a Taylor series around parameters a1, b1, a2, and b2. The crucial role is played by its prop-
aw = 0 as erties at zero water activity. The value of aw/w at this point is equal
74 J. Blahovec, S. Yanniotis / Journal of Food Engineering 91 (2009) 72–77
to A/D = a1a2/(a1 + a2). The first derivative at the same point is Comparing the inequality (6a) with inequality (5b) it is clear that
given then as the turning point can be formed only with an initially increasing
aw function for aw/w, and this turning point is maximum when it is ob-
d w B AE a2 b1 a21 b2
¼ ¼ X 02 ¼ 2 ¼ D10 ð5aÞ served (Blahovec and Yanniotis, 2007).
daw 0 D D2 ða1 þ a2 Þ2 In the general case (b1 – b2), the maximum is given by the
This value is positive, i.e., the function aw/w is an increasing one, if following formula
2 sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi3 " sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi#
a22 b1 a21 b2 ð5bÞ 1 4 X 4 X 02 5 1 X 4 D10
awm ¼ 1 1 ¼ 1 1 ð6cÞ
X4 X3 X4 X3
or alternatively if
X2 X1X4 ð5cÞ where D10 is first derivative of aw/w at aw = 0 given by Eq. (5a).
There exists a simple relation between the first derivatives of w
The function is decreasing when the opposite inequalities to Eqs.
and aw/w vs. aw
(5b) and (5c) are fulfilled. When b1 = b2, the function at the zero
point is increasing if a2 > a1 and vice versa. dw w d aww
The first derivative of Eq. (2f) is given by ¼ 1w ð7Þ
daw aw daw
d aww X 0 2X 3 aw X 3 X 4 a2w
¼ 2 ð6Þ which indicates that for positive w and aw, the negative (aw/w)
daw ð1 þ X 4 aw Þ2 derivative is followed by increase in w vs. aw. For positive values
which for E = 0 (i.e., b1 = b2 = b) is of the derivative of (aw/w), the w derivative is less than the ratio
w/aw. When the (aw/w) derivative is zero, the w derivative is
d aww b w/aw, so that the tangent to the usual sorption isotherm at this
¼ X 2 2X 3 aw ¼ ða2 a1 2baw Þ ð6aÞ
daw a1 þ a2 point is the line going through the initial values (w = aw = 0).
The plot aw/waw has a mathematical extreme (or a turning point) The shapes of the plots of aw/w vs. aw are given in Fig. 1. Fig. 1a
at water activity awm if Eq. (6a) is equal to zero for awm in the usual shows the influence of the parameters a1 and a2. For lower param-
range h0,1i, i.e., when the following inequalities are fulfilled eters a2 the lower initial slopes of aw/waw plots are observed in
agreement with Eq. (5a). The greater the value of b1 the greater
B a2 a1 is the slope of the plot.
0 a2 a1 2b; awm ¼ ¼ ð6bÞ
2C 1 2b
4. Classification of the sorption isotherms
6 formulae given by Eqs. (4a)–(4d), (4f) and (4g). The initial deriva-
aw/w
tive of aw/w vs. aw is calculated from Eq. (5a). When this value is
less than or equal to zero, the sorption isotherm can be classified
4 as solution-like (III class of the Brunauer’s classification). For high-
er values of water activity, the slope of the ratio aw/w vs. aw dec-
reases in its negative values, so that, in agreement with
2 discussion following Eq. (7), the slope of moisture content (w) vs.
0 0.2 0. 4 0.6 0. 8 1
water activity (aw) will increase with increasing water activity
Water Activity (-) which is typical for solution behaviour described by the Raoult’s
law.
1-1-1-2
b 0.6 When the initial aw/w derivative is positive, we can have two
1-1-5-1 important classes of isotherms: the Langmuir-like isotherms (I
0.5 1-1-1-1 class of the Brunauer’s classification) and GAB-like isotherms (II
0.4
1-1-5-5 class of Brunauer’s classification). In the case of Langmuir’s-like
aw /w (-)
from the other two types, but its numerical value can be under-
stood as a measure of the special character (consisted in solution
a 0.050
and/or surface forces). This quantity is denoted as D10 and it is
given by Eq. (5a). The last important parameter is the ratio of the 0.040
first derivative of the aw/waw plot at the final value (i.e., at
aw = 1) to the first derivative at the initial value (at aw = 0), denoted 0.030
aw/w
as Rfi that is given by Eqs. (5a) and (6) Type I
0.020
1 X 3 2þX
X 02
4
Type III
Rfi ¼ 2
: ð8Þ
ð1 þ X 4 Þ 0.010
0.150 X4
-2
99.9
0.050 -3 99
95
-4 Approximation
0.000
0.0 0.2 0.4 0.6 0.8 1.0 -5
Water Activity
-6
30
-7
Moisture Content (% db)
25
Type IIa Fig. 5. Ratio of the final to the initial slope of aw/waw plot – Rfi from Eq. (8) plotted
against parameter X4 for 75 sorption isotherms from literature (see text). The
20 Type IIb numbers in the legend denote minimal coefficients of determination in the sets
Type IIc expressed in percent. The plot is approximated by the following expression
15 Rfi = A(X4 + B)n, where A = 1.1462 ± 0.1891, B = 1.1589 ± 0.1199, n = 1.3719 ±
0.3203 are parameters (R2 = 0.851).
10
value at which a similar maximum is observed for the case X4 = 0.
5 The experimental data in Fig. 6 are plotted using a similar power
formula with the argument approximately equal to 1 + X4. We can
0 then divide the sorption isotherms into three classes: class IIa rep-
0 0.2 0.4 0.6 0.8 1 resented by nearly classical GAB sorption isotherms; they are iso-
Water Activity therms with X4 close to zero: 0.1 < X4 < 0.1, the type IIb with
X4 < 0.1; and the type IIc with X4 > 0.1 (see also Fig. 3). Type IIb
Fig. 3. The characteristic GAB-like isotherms. Type IIa is close to the standard GAB
isotherm: 0.1 6 X4 6 0.1 – the sorption isotherm for adsorption of chicken at
is closer to the Langmuir-like isotherms at lower water activities
60 °C – Wolf et al. (1972), R2 = 0.999, D10 = 0.245, Rfi = 1.177, X1 = 0.0181, and type IIc is closer to the solution-like isotherms at higher water
X4 = 0.0738, awm = 0.433; type IIb is typical by X4 < 0.1 – desorption of soya bean activities. The subtype IIc is sometimes observed in the case of fruits
at 70 °C – Aviara et al. (2004), R2 = 0.997, D10 = 0.122, Rfi = 5.494, X1 = 0.0037, and vegetables (e.g., pineapple in Fig. 4). X4 expresses the combined
X4 = 0.8228, awm = 0.709; type IIc is typical when X4 > 0.1 – adsorption of Pecan
effect of parameters a1, a2, b1 and b2 and its sign depends on the rel-
nut at 25 °C – Wolf et al. (1972), R2 = 0.998, D10 = 0.596, Rfi = 0.247, X1 = 0.0289,
X4 = 1.4009, awm = 0.516. (a) aw/w plotted against water activity, (b) the standard ative magnitude of b1 and b2. High monolayer values correspond to
plot of the sorption isotherm (moisture content d.b. vs. water activity). low values of b1 and negative X4 (Langmuir-like isotherms). Low
monolayer values correspond to high b1 and positive X4 (solution-
like isotherms). The basic characteristics of sorption isotherms
0.10 according to the criteria developed in this paper are summarised
in Table 1. In summary, the proposed equation describes sorption
0.08 isotherms in the whole range of water activity (0–1) successfully
Experiment
(Fig. 7) and can be used for quantitative classification of sorption
0.06 Approximation
isotherms. More detailed analysis of experimental isotherms will
be published separately (Yanniotis and Blahovec, submitted for
aw/w
0.04 publication).
0.02
3.5
0.00
3.0
Relative awmax
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