Journalof Food Engineering14 (1991) 269-287

Moisture Sorption Isotherm Characteristics of Potatoes at Four Temperatures

N. Wang & J. G. Brent-m
Department of Food Science and Technology, University of Reading, Whiteknights, PO Box 226, Reading RG6 2AP, UK 1990;

(Received 14 June 1990; revised version received 20 November accepted 22 November 1990)

ABSTRACT Moisture equilibrium data of potatoes by desorption and adsorption were determined at 40, 50, 60 and 70C. The experimental procedure was a gravimetric method. Isosteric heats of water desorption and adsorption were calculated by applying the Clausius-Clapeyron equation to the sorption isotherms at diflerent temperatures. Seven mathematical models were used to fit the experimental data. A nonlinear least-squares regression program was used to evaluate the constants of the seven desorption and adsorption isotherm models.

INTRODUCTION The importance of sorption isotherm data in considering drying problems is evident. Drying is a combined heat and mass transfer process, in which the product temperature rises from room temperature and approaches the drying air temperature. The sorption data may be used for the proper choice of the end-point of drying process (Gal, 1987), that is the optimum residual moisture content of the final product. Too high a residual moisture content after too short a drying time leads to reduced stability, whereas reduction of the final moisture content below its optimum value wastes energy in the operation. Another application of sorption isotherms is in the calculation of the drying time of hygroscopic substances (Gal, 1987). The differential heat of sorption is a useful quantity because it yields information on the energetics of water sorption processes in foods. The
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Journal of Food Engineering 0260-8774/91/$03.50 - 0 1991

Elsevier

Science

Publishers Ltd, England. Printed in Great Britain

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level of moisture content at which the differential heat of sorption approaches the heat of vaporization of water is often taken as indicative of the amount of bound water existing in the food (Duckworth, 1972). Knowledge of the differential heat of sorption is very important when designing equipment to be utilized in dehydration processes (Becker & Sallans, 1956; Heldman et al., 1965). The heat of vaporization of sorbed water may increase to values well above the vaporization of pure water as food is dehydrated to low moisture levels. The general case of drying of food materials involves energy input to remove free water through sublimation or evaporation and water associated with the food matrix (Rizvi, 1986). Values of isosteric heats of adsorption were reported for spray-dried eggs by Makower (1945); for wheat (desorption) by Becker and Sallans (1956); for wheat flour, starch and gluten (adsorption) by Bushuk and Winkler (1957); for maize (desorption) by Rodriguez-Arias et al. (1963) and Chung and Pfost (1967a); for freeze-dried starch, gelatin gel, beef and peach (adsorption) by Saravacos and Stinchfield (1965). Iglesias and Chirife (1976a, b) obtained values of the isosteric heat of water adsorption and desorption of several foods, including fruits, protein foods, vegetables and spices. The objectives of this work are (a) to obtain data on desorption and adsorption isotherms of potato between 40 and 70C; (b) to report the isosteric heat of water sorption; and (c) to evaluate constants of sorption isotherm models, using nonlinear least-squares regression analysis. MATERIALS Materials Fresh Desiree potatoes were purchased from a local market and kept in a cold room at 10C for about 2 weeks prior to their use. Fresh potatoes were used in desorption experiments. Samples used in adsorption experiments were sliced to 1-mm thickness, frozen at - 18C and freezedried for 24 h to attain a low moisture content (Gutierrez-Lopez, 1989). Determination of sorption isotherms A gravimetric technique was used to determine the equilibrium moisture content of potatoes at several temperatures. Duplicate samples each of 3 g + 0.00 1 g for desorption and O-3 g + 0.000 1 g for adsorption were placed in petri dishes which were placed inside sorption jars. Sulphuric AND METHODS

Moisture sorption isotherms ofpotatoes

271

acid solutions were used to maintain the relative humidity inside the jars. The jars were kept in temperature-controlled cabinets which were set at 40,50,60 and 70C. The cabinet temperatures were monitored and controlled within + 1C. The concentrations of sulphuric acid at different temperatures are listed in Table 1 together with literature values for their relative humidities (Gutierrez-Lopez, 1989). Sample were equilibrated for 3 weeks or more to constant weight ( + 0.0001 g). The weight of dry matter was determined by drying at 70C under vacuum for 24 h. Models for fitting to sorption isotherm data The equilibrium moisture data were fitted with seven mathematical models shown in Table 2. The nonlinear regression analysis (SAS, 1982) was used to estimate the constants of the models from the experimental results. To evaluate the goodness of fit of each equation, the mean relative percentage deviation modulus (E) was used (Aguerre et cd., 1989). This modulus is defined by the following equation: 100 ~ InZi-m,jI E% = N i=l mi

(1)

where lzti and mPi are experimental and predicted values, respectively, and N is the number of experimental data. This parameter was used in the literature to evaluate the goodness of fit of different mathematical expressions as applied to experimental data (Boquet et al, 1978; Lomauro et al., 1985). It is generally considered that E values below 10% indicate a reasonably good fit for practical purposes.

TABLE 1

Relative Humidities of Sulphuric Acid Solutions at the Temperatures Used Temperature CC) 40 50 60 70 % (w/w) Sulphuric acid 20 88-l 88.2 88.3 88.4 30 75.8 76.2 76.6 77-o 40 57.7 58.5 59-3 60.1 50 37.3 38-3 39.4 40-5 55 27-4 28.5 29.6 30.6 60 18.0 19.0 20-o 20.9 65 11.0 11.8 12.7 13.5 70 4.8 5.4 6-2 6.8

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TABLE 2 Models for Fitting the Sorption Isotherms of Potatoes

Name of model Models

GAB (Van Den Berg & Bruin, 198 1) Chen (Chen, 1971) Oswin (Oswin, 1946) Chung-Pfost (Chung & Pfost, 1967b) Henderson (Henderson, 1952)

M= CKMoA,/[( 1 - KA,)( 1 - KA, + CKA,)]

A, = exp[A- B exp( -CM)]

M= A(A,/( I - A,)lB
A, = exp[ - A/T exp( - BM)] A, = 1 - exp( ATMB) A, = exp( -A/MB) M=hIoCA,/[(l-A,)+(C-l)(l-A,)A,]

Halsey (Halsey, 1948) BET (Brunauer etal., 1938)

A, B, C and K =constants in sorption isotherm models; A,=water activity; M = moisture content (dry basis); MO = monolayer moisture content (dry basis); R = gas constant (k&/mole K); T= absolute temperature (K).

Determination of the isosteric heat of sorption The application of the Clausius-Clapeyron equation to the isosteric equilibrium pressures at different temperatures (sorption isotherms) is a widely used procedure for the calculation of the isosteric heat of sorption (e.g. Peri & De Cesari, 1974; Mazza & Le Maguer, 1978). The isosteric heat of sorption is a differential molar quantity derived from the temperature dependence of the isotherm (Iglesias & Chirife, 1976~) (dm P/dT),, = Q/RT*
(2)

where QSfis the isosteric heat of sorption (k&/g mole), T is the temperature, R the gas constant and P is the partial pressure vapour or equilibrium vapour pressure of the sorbate. At a amount of sorbed water (yla), the Clausius-Clapeyron equation water is dm P,,/dT= L/RT2

absolute of water constant for pure

(3)

Moisture sorption isothenm of potatoes

273

where L is the latent heat of vaporization at the specified temperature (average temperature between 40 and 70C) and PO the saturation pressure at temperature T. Substracting eqn (3) from eqn (2) [dln(P&)/dT],,.=(dlnA,/dT),=Q;/RT2 (4) where A, is the water activity and Q;rtthe net isosteric heat of sorption. The net isosteric heat of sorption, at any value of nu, may be calculated from eqn (4) by plotting the sorption isotherm as In A, versus 11 T and determinin g the slope, which equals - Qf /R. By this method it is assumed that Q;l is invariant with T, but the application of this method requires the measurement of sorption isotherms at more than two temperatures. The isosteric heat may also be calculated from the integrated form of eqn (4) applied to sorption isotherms measured at two temperatures:

QZ = R[( Tl Tz)/( Tz - ?)I bb%v, /A,~ )I

(5)

The isosteric heat is reported in the manner used by Iglesias and Chirife (1976a), that is in the form of a plot of Q versus moisture content. The Q was calculated as
Qs=Qit+L, (6)

where L, is the latent heat of vaporization of pure water for desorption or the heat of condensation of pure water vapour for adsorption at the specified temperature (55C, average between 40 and 70C). Young and Crowell(1962) and Ross and Olivier (1964) reviewed the quantitative relationships between the isosteric heat of sorption and other experimentally determined heats of sorption, like adiabatic and isothermal calorimetric heats and the integral heat of sorption. In this work, eqn (4) was used to calculate the isosteric heats of sorption. A least-squares analysis was performed to obtain the slope of the straight line representing ln A, versus l/ T. The isosteric heats reported here were obtained from sorption isotherms which show marked hysteresis. However, this procedure may be questioned, since in systems exhibiting hysteresis either the adsorption branch or the desorption one, or both, must involve thermodynamically irreversible phenomena. Evenett and Whitton (1955) suggested that, in systems exhibiting hysteresis, the Clausius-Clapeyron equation may have the form

dh P ___ [ d(l/T)

1
na

= AH + Q = AH(apparent) R
R

(71

274

N. Wang, J. G. Brennan

and desorption, AH is the calorimetric isosteric heat of adsorption (or desorption) and Q is the so-called uncompensated heat (which in an isothermal irreversible process is related to the entropy production (d,S) arising from the irreversibility, Q = T(diS); therefore, the isosteric heat does not strictly refer to heat transfer of the sorption process). Evenett and Whitton ( 1955) also suggested that if eqn (7) was valid, by combining isotherm measurements with calorimetric measurements of the heat of adsorption, it should be possible to decide which part of the isotherm cycle is associated with an irreversible process. The measurements require high precision through strict and difficult control of experimental variables, due to the small value of (2. From a practical standpoint, Iglesias and Chirife (1976a) concluded that the heats of changes involved in irreversible processes are probably small compared with the overall energy changes, so they may be neglected in a general qualitative description or in the estimation of heat requirements for the dehydration process. Accordingly, they added that the apparent heats of sorption calculated from the conventional Clausius-Clapeyron equation will be adequate for a qualitative thermodynamic discussion of the adsorption and desorption processes.

is the apparent differential molar heat of adsorption whereAHtapparenr)

RESULTS AND DISCUSSION Desorption and adsorption isotherms The desorption and adsorption isotherms at 40, 50, 60 and 70C are shown in Figs 1 and 2. The points shown are average values from three determinations and coefficients of variation range from 1.5 to 5.4%. The equilibrium moisture contents increase with decrease in temperature at constant water activity, and increase with rise in water activity when temperature was kept constant. The sorption isotherms give the characteristic S-shaped curve, typical of many sorption isotherms of food (Iglesias & Chirife, 1982). Figure 3 shows that hysteresis between desorption and adsorption is exhibited over almost the entire range of relative humidity. Heats of desorption and adsorption When water vapour is adsorbed on a surface, a quantity of heat (the heat of adsorption) is released. When adsorbed water vapour is desorbed, a quantity of heat is taken up (the heat of desorption) and is a measure of

Moisture sorption isotherms of potatoes 30 7oc 60-c 50-c

275

0.0

0.2

0.4

0.6

0.8

1.0

Water

activity

Fig. 1.

Desorption

isotherms of potatoes at different temperatures.

I-

40% 50-c 60-c 70-c

0.0

0.2

0.4

0.6

0.8

1.0

Water

activity

Fig. 2.

Adsorption

isotherms of potatoes at different temperatures.

the heat or energy that must be added to the adsorbed gas to break the intermolecular force (Chung & Pfost, 1967~). The heats of desorption and adsorption indicate the binding energy or the intermolecular force between the molecules of water vapour and the surface of adsorbent. Water sorption in foods is a complex phenomenon, The main watersorbing constituents of foods are various polymers (proteins, starch, cellulose, hemicellulose, etc.) and sugars. The different polar groups of the polymers provide energetically different preferential sites for the

276

N. Wang, J. G. Brennan

0.0

0.2

0.4

0.6

0.8

1.0

-I
0.4 Water 0.6 activity 0.8 1.0

Fig. 3. Desorption

and adsorption

isotherms of potatoes at hysteresis effect.

40C and 70C showing

water. Besides, as a polymer sorbs water it undergoes changes of constitution, dimensions and other properties (McLaren & Rowen, 1951; Masuzawa & Sterling, 1968). Water sorption also leads to phase transformations of the sugars contained in the food (IgIesias et af., 1975). Ah these facts make difficult the interpretation of the differential heat curves; there are, however, some observations that could be made from the results.

Moisture sorption isotherm

ofpotatoes

277

18 r^ 5

__-_

HeuofdaorpQn Latent heat Heat of adsorption

.
T

i!

3 *o 0

14

.
12

!z
%

. a * = loS!. 0

_-_--___-_-_-_--_ I.
2

I.
4

t.1.1.
6 8 10

I.
12

I.
14

1.1.
16 I8

I
20

Moisture content (% dry basis)

Fig. 4.

Isosteric heats of desorption

and adsorption

for potatoes at 55C.

The isosteric heats of desorption and adsorption are plotted as a function of moisture content in Fig. 4. Plots of heats of desorption and adsorption demonstrate that heats of sorption decrease continually with increasing moisture content. The horizontal dotted line indicates the heat of vaporization of pure water or heat of condensation of pure water vapour at 55C (the average temperature between 40 and 70C). The decrease in the isosteric heats with amount of water sorbed can be qualitatively explained by considering that, initially, sorption occurs on the most active available sites giving rise to high interaction energy. As these sites become occupied, sorption occurs on the less active sites, giving rise to lower heats of sorption (Iglesias & Chirife, 1976~). It can also be seen from Fig. 4 that the isosteric heats of desorption and adsorption at very low moisture content are still higher than the heats of vaporization and condensation of pure water. McLaren and Rowen (1951) pointed out that the chemisorption on polar groups could be responsible for the higher sorption heat at very low moisture content. In studying the sorption of polar vapours on cellulose fibres, Colombo and Immergut (1970) observed an abnormahy high heat of sorption at low coverages indicating the presence of high-energy sites, which they attributed to strained hydrogen bonds induced in the fibre on drying. Upon sorption these strained hydrogen bonds were broken with a net evolution of heat, in addition to the heat evolved from the formation of stable hydrogen bonds between the cellulose and the vapour. An effect of this type could partially account for the high initial heats observed in Fig. 4. Another observation from Fig. 4 is that the values of isosteric

278

N. Wang,J. G. Brennan

heats of desorption are greater than those of adsorption, indicating that energy involved in the desorption process is greater than that in the adsorption process. Iglesias and Chirife (1976~) compared the isosteric heats of water adsorption and desorption for a large number of foods. In general, the desorption heats were significantly higher than the adsorption heats at low moisture contents. Upon further sorption, the difference rapidly decreased and practically disappeared at high moisture contents. They concluded that there was no direct relationship between the observed differences in the adsorption and desorption heats and the distribution of hysteresis along the sorption isotherm. Several theories have been advanced to explain the phenomena of hysteresis. If hysteresis arises from a capillary condensation mechanism, two theories exist to explain the form of the isotherm. These are the ink-bottle theory of Kraemer ( 193 1) and McBain ( 193 5), and the delayed meniscus theory of Foster (1932) and Cohan (1938). It is believed that it is not possible to give a single explanation of the hysteresis phenomena in foods; each food is a complex combination of various constituents which not only can sorb water independently, but can also interact among themselves giving rise to different water-sorbing capacities. The existence of higher values of desorption heats as compared with adsorption heats may be due to structural modifications which take place on the substrate during desorption, modifying the overall energy of binding of the sorbate through co-operative binding or to entrapment effects. Rao (1942) attributed such changes of sorption phenomena, resulting in the elimination of hysteresis, to the elastic properties of organogels. In sorption, the capillary pores of the adsorbent become elastic and swell. Upon desorption, the removal of water causes shrinkage and a general collapse of the capillary porous structure. Alteration of structure causes elimination of hysteresis due to the absence of capillary condensation. When considering the application of the Clausius-Clapeyron equation, it is obvious that anything that affects the sorption isotherm affects the thermodynamic quantities derived from it; this includes the prehistory of the sample, such as various preheat treatments, blanching, freezing and drying. The treatment may change the polar and other groups that bind water, along with changes in capillary and other configurations of the food structure (Kapsalis, 1987). According to Chung and Pfost (1967a), the heats of sorption can be considered as indicative of intermolecular attraction forces between sorptive sites and water vapour. Plotted values of Q versus moisture content can be used to study the magnitude of the binding energy or the availability of polar sites to water vapour as sorption proceeds. Figure 4

Moisture sorption isotherms of potatoes

279

TABLE 3 Parameter Values for all Models in Desorption Model 40 GAB C K MO E (%) Chen A B C E (%) Oswin A B E (%) Chung-Pfost A B E (%) Henderson A B E (%) Halsey A B E (%) BET C MO E (%) A, range (%) BET All others Temperature (C) 50 60 70

12.52 0.84 0.059 5.68 - 0.097 4.37 21.26 10.14 0.092 0.44 4.27 1 188.89 17.46 16.09 0.084 1.57 13.34 0.049 0.92 115.82 19.54 0.047 7.33 4.8-57.7 4.8-88.1

8.89 0.82 0.06 1 6.74 - 0.104 4.08 22.00 11.18 0.087 044 5.41 1 138.08 17.63 17.04 0.075 1.49 13.52 0.046 0.92 105.00 16.71 0.045 6.11 5.4-58.5 5.4-88.2

8.57 0.84 GO53 4.59 -0.111 3.95 24.27 8.09 0.078 0.46 3.67 1119.92 18.95 15.28 0.075 1.44 11.54 0.042 0.94 81.09 14.65 0.04 1 4.78 6.2-59.3 6.2-88.3

4.37 0.80 0.057 9.15 - 0.094 3.15 23.44 15.78 0.068 0.49 9.13 991.49 19.22 19.47 0.06 1 1.29 14.30 0.041 1.03 9.82 7.99 0.038 8.71 6.8-60.1 6.8-88.4

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N. Wang, J. G. Brennan

TABLE 4 Parameter Values for all Models in Adsorption

Model 40
GAB c K $h) Chen A B C

Temperature (C) 50 60 70

13.73 0.83 0.052 5.62 - 0.083 4.47 23.79 9.92 0.082 0.43 4.13 1243.12 20.24 14.72 0.117 1.62 13.39 0.0025 2.64 70.35 11.79 0.049 7.83 4.8-37.3 4.8-88.1

13.41 082 0.048 4.08 - 0.086 4.60 27.06 7.24 0.074 0.42 3.31 1301.08 22.78 11.93 0.142 1.64 10.58 0.002 1 2.6 1 71.00 11.52 0.043 4.50 5.4-38.3 5.4-88.2

21.18 0.86 0.036 3.41 - 0105 5.46 35.90 4.63 0062 0.43 4.07 1 466.60 28.73 9.15 0.22 1 1.72 12.69 0.0017 2.50 69.82 14.69 0037 3.08 6.2-39.4 6.2-88.3

17.75 0.90 0.029 5.69 - 0.109 4.26 38.59 10.97 0051 0.49 586 1 244.86 3077 16.50 0.170 1.58 15.66 0.0012 2.49 70.27 14.82 0.028 6.19 6.8-40.5 6.8-88.4

E (%)
Oswin A B

E (%)
Chung-Pfost A B

E (%)
Henderson A B

E (%)
Halsey A B

E (%)
BET C

MO E (%) A, range (%)

BET All others

Moisture sorption isotherm of potatoes

281

Adwqxion _._.&_.

GAB

at WC

Expcrimd Rediued

0.0

0.2

0.4 water

0.6 activity

0.8

1.0

Fig. 5.

Comparison between experimental and predicted values using GAB equation at 60C.

also shows that the heats of sorption approach the latent heat of vaporization or condensation at 55C as the moisture content increases, indicating that adsorbed water vapour on the adsorbent may behave like pure water at either higher moisture content or higher relative humidity. Iglesias and Chirife (1976~) analysed the differential heat curves for adsorption. They stated that an isosteric heat value greater than the heat of condensation indicates that the energy of interaction between the

282
30-

N. Wang, J. G. Brennan Dcmptiml oswm .L6oT Expaimmtal _._.&_. Rediced

0.6

0.8

0.0

0.2

0.4

0.6

0.8

1.0

Fig. 6.

Comparison

Water activity between experimental and predicted values using Oswin equation at 60C.

sorbate sorbate The potato Chirife

and sorption sites is greater than the energy that holds the molecules together in the liquid state. values of the isosteric heats of desorption and adsorption of were compared with those of vegetables reported by Iglesias and ( 1976~): a good agreement was found.

Fitting of equations to sorption isotherm data The estimated constants and the mean relative deviation modulus (E) for the models in Table 2 are presented in Table 3 and Table 4. It can be

Moisture sorption kotherm

of potatoes

283

seen that GAB and Oswin equations give smaller mean relative percentage deviation (less than 10%); therefore, they give the best fit to the experimental data for a wide range of water activities (O-88*4%). The results agree with those reported by Aguerre et al. (1989). Moreover, it is found that the BET equation gives a better fit to the experimental data for desorption of potato in the range of water activity 0.05-O-60, and for adsorption in the range of water activity 0.05-0.40. For adsorption, there is a good agreement with Chirife and Iglesias (1978), who stated that the BET equation usually holds only between water activity from about 0.05

0.6

0.8

Warn

activity
BlT .t WC

-1 -

Adsmption

0.6

0.8

Fig. 7.

Comparison between experimental and predicted values using BET equation at 60C.

284

N. Wang, J. G. Brennan

to 0.45. For desorption, the water activity range is slightly larger than this range (o-0.45). It is obvious that the Halsey equation gives a poor fit to the data. However, this is different from the conclusion reached by Boquet et al. (1978). They concluded that the Halsey equation gave a better fit for vegetables. Examples of the comparisons between experimental and predicted values at 60C using GAB, Oswin, BET and Halsey equations are shown in Figs 5-8.

30 DcmrptimHALSEY at WC 25-

Expaimslul Pdictcd

_._.&_.

0.4 Water

0.6 activity

Fig. 8.

Comparison between experimental and predicted values using Halsey equation at 60C.

Moisture sorption isotherms of potatoes

285

CONCLUSIONS From the experiment, the following may be concluded.

(1) Temperature has an effect on sorption isotherms. The equilibrium moisture content increases with decreasing temperature at constant water activity. The water activity increases with increase in temperature when the moisture content is kept constant. This behaviour is typical of many foods. (2) The isosteric heats of sorption increase with decreasing moisture content. The heat of desorption is greater than that of adsorption at low moisture contents. At higher moisture contents the difference tends to disappear. (3) The GAB and Oswin equations are suitable for representing the relationship between water activity and equilibrium moisture content of potato in the range of water activity O-88%, and the BET equation in the range of water activity O-60%. This work represents the preliminary stage of a study of the convective drying of potato and the solid-moisture relationships involved.

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u-technol., 22, 192-5. Becker, H. A. & Sallans, H. R. (1956). A study of desorption isotherms of wheat at 25 and 50C. Cereal Chem., 33,79. Boquet, R., Chirife, J. & Iglesias, H. A. ( 1978). Equations for fitting water sorption isotherm of foods. II. Evaluation of various two-parameter models. J. Food Technol., 13,319-27. Brunauer, S., Emmett, P. H. & Teller, E. (1938). Adsorption of gases in multimolecular layer. J. Amer. Chem. Sot., 60,309-19. Bushuk, W. & Winkler, C. A. (1957). Sorption of water vapor on wheat flour, starch, and gluten. Cereal Chem., 3473. Chen, C. S. (1971). Equilibrium moisture curves for biological materials. Trans. ASAE, 14,924-6. Chirife, J. & Iglesias, H. A. ( 1978). Equations for fitting water sorption isotherms of foods. Part I. A review. J. Food Technol., 13,159-74. Chung, D. S. & Pfost, H. B. (1967a). Adsorption and desorption of water vapor by cereal grains and their products. Part I. Heat and free energy changes of adsorption and desorption. Trans. ASAE, 10,549-5 1. Chung, D. S. & Pfost, H. B. (19676). Adsorption and desorption of water vapor by cereal grains and their products. Part II. Development of the general isotherm equation. Trans. ASAE, 10, 552-5.

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