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LWT 41 (2008) 13101316 www.elsevier.com/locate/lwt

Hydration of grain kernels and its effect on drying

Richard S. Ruiz, Mario G. Vizcarra, Carlos Mart nez
noma Metropolitana-Iztapalapa, Av. San Rafael Atlixco 186, Col. Vicentina, 09340 Me xico, D.F., Mexico Area de Ingeniera Qumica, Universidad Auto Received 2 October 2006; received in revised form 16 July 2007; accepted 23 August 2007

Abstract Different hydration methods have been considered and their effect on the drying characteristics of corn and amaranth grains have been studied at different drying temperatures and the results compared with those for the fresh materials. The effect of hydration on drying was found to depend on the type of grain. In general, for corn hydrated grain particles the moisture content was found to be in a looser condition than it was in the fresh grains, and hence, smaller effective diffusion coefcients where found for the latter. Such differences were found to increase with increasing drying temperature. Also a rst-order irreversible kinetic model was applied to the drying data for hydrated and fresh corn and a reduction on the drying activation energy was observed by the humidication process. In contrast, for the relatively small amaranth grains, both hydrated and fresh particles showed similar drying characteristics. The results suggest that drying kinetics and transport properties obtained for rehydrated grains can overestimate drying rates for the corresponding freshly harvested material, especially at relatively high moisture contents and for relatively large grain particles like corn. r 2007 Swiss Society of Food Science and Technology. Published by Elsevier Ltd. All rights reserved.
Keywords: Hydration method; Drying characteristics; Diffusion; Activation energy; Corn; Amaranth

1. Introduction It is often found that drying studies of cereal grains reported in the literature have utilized rewetted particles instead of the fresh material. This seems to be common practice when freshly harvested grains are not available for the desired study. The impact of using a rewetted material on the drying phenomena and on the characteristics of the dried particles has been reported in some studies (Campa na, Sempe, & Filgueira, 1993; Devahastin, Mujumdar, & Raghavan, 1998; Mart nez-Vera, Ruiz-Mart nez, & Viz carra-Mendoza, 2005; Mourad, Hemati, & Laguerie, 1995; Tosi & Re, 1999). Many of the works that have used hydrated materials have also reported little difference between the drying behavior of fresh and hydrated grains while other researchers do report an effect. For instance, one has that Mourad et al. (1995) compared the drying kinetics of fresh and rewetted yellow dent corn particles obtained in a uidized bed and reported no practical difference between both of them. Beke, Mujumdar, and
Corresponding author. Tel.: +52 5 8044648.

E-mail address: rmr@xanum.uam.mx (R.S. Ruiz).

Bosisio (1995), in contrast, studied the drying of fresh and rewetted yellow dent corn under microwave conditions and reported slower drying rates for the fresh material. From a comparison of both of these works, at least, it is found that the rewetted materials have been prepared using different hydration methods. There are some other works that have employed rewetted grains as representative of fresh grains or seeds but that do not seem to consider the possible effect of doing so on their drying results. Several methodologies have been used in the literature for preparing rewetted materials and among which the following are commonly utilized. Grain particles are often rewetted by immersion in water during different periods of time depending on the initial moisture content that wants to be attained. Other researchers rewet particles by contacting the mass of grains to be rewetted with the exact amount of water required to reach the desired initial moisture content. Another methodology used considers rewetting of the particles by placing them within an environment of saturated air for the time necessary for them to reach the moisture content of interest. In a previous work (Mart nez-Vera et al., 2005), a comparison of the effect on the drying characteristics of

0023-6438/$34.00 r 2007 Swiss Society of Food Science and Technology. Published by Elsevier Ltd. All rights reserved. doi:10.1016/j.lwt.2007.08.007

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cereal grains humidied by different methods was reported. In such work, however, the initial moisture contents considered were in many cases signicantly lower than those for the fresh materials, an important limitation to reaching to possible conclusions. From this, an evaluation of the impact of the rehydration process for moisture contents typical of the fresh grains appears to be missing, therefore, in order to identify possible drawbacks associated with the use of hydrated grains to model fresh grain drying behavior, in the present work the effect of the procedure followed for hydrating grain particles on their drying process has been studied for amaranth and corn grains and compared with the observed drying characteristics for the fresh materials. 2. Materials and method Fresh and hydrated amaranth (Amaranthus hypochondriacus) and corn (Zea mays) grains were utilized in the present work. The materials employed were collected in the central part of Mexico, directly from the growing eld. Due to their relatively high initial moisture content and in order to avoid product deterioration, drying curves for the fresh materials were determined shortly after harvesting. The dried grains were obtained from the fresh material, which was dried slowly by placing and keeping the sample in a closed chamber with dry air (10% RH at room temperature) for at least 21 days. Particles were then moistened by three different methods: in one of them particles were placed in an isothermal chamber with air at 82% relative humidity and 294 K temperature, and left to moisten for periods of time of up to 7 days; in the second procedure grains were soaked in water at 291 K by immersing the grain sample in distilled water for periods of 24 and 48 h; and in the third method the grains are put in contact in a closed container and mixed thoroughly with the exact amount of distilled water (at 291 K) required to achieve a desired initial moisture content. For the last two methods, conditioning periods at 4 1C of up to 72 h were considered, in which the grain samples were placed in a sealed plastic container and kept in cold storage so as to promote moisture absorption and distribution within the kernels. The drying curves for the fresh and rewetted grains were then determined by irradiative drying with an OHAUS moisture determination balance at different temperatures in the 40100 1C range. The balance provides uniform infrared heating with a fast response time (test area reaches full temperature in less than 1 min). In a typical drying run, the balance is set to a given temperature and drying time, a 10 g sample is placed in a 0.09 m diameter aluminum pan with the kernels uniformly distributed as a monolayer, after which the drying experiment is initiated and the weight change is recorded as a function of time. The initial moisture content was determined by drying the samples in an oven at 103 1C for 72 h (Ramos, Pezet-Valdez, OCon nor-Sanchez, Placencia, & Pless, 2004). To determine the drying rate at a given moisture content the drying curve

data was locally tted to a third grade polynomial by nonlinear regression, such equation was then differentiated with respect to time and the resulting expression was evaluated at the moisture content of interest. 3. Results and discussion 3.1. Drying curves For a rewetted material, its initial moisture content as well as the characteristics of its drying curve are expected to be affected by the hydration procedure utilized. Fig. 1(a) shows the drying curves for fresh and hydrated corn using three different hydration methods. As can be seen in this gure, it seems that the initial moisture content of fresh corn can be reproduced by rewetting dried corn kernels with liquid water. Although in Fig. 1(a) the initial moisture contents of grains hydrated by soaking the sample or by addition of water are somewhat smaller than the value for fresh corn (0.79 kg water/kg db initial moisture content for fresh corn), it was observed that the moisture absorbed could be increased by increasing the soaking and conditioning times. The method of hydration by contact with humid air was found to be relatively slow and therefore inadequate since the grain was prone to mold attack. It is evident from Fig. 1 that the drying curves for the hydrated materials suggest faster drying rates when compared with that for fresh corn. Drying curves for fresh and hydrated amaranth are presented in Fig. 1(b). For grains hydrated by addition of water the initial moisture content of the fresh material is attainable as long as the proper amount of water is used. As was found for corn, the hydration of amaranth grains by contact with humid air was a relatively slow process that makes the grain prone to germination or to mold attack and, therefore, after 7 days of hydration only 29% db moisture content could be attained compared to 40% for the fresh grains. In contrast with what was observed in Fig. 1(a) for corn grains, and regardless of the initial moisture content of amaranth grains, the drying curves for fresh and hydrated materials seemed to be qualitatively similar between each other. The drying rate of rewetted solids can be affected by the way in which moisture is introduced into the solid structure and identication of such effects is presented in Fig. 2. The time variation of moisture content for fresh corn and for grains hydrated by soaking in water are presented in Fig. 2(a). These curves were obtained from drying curves at 80 1C and the rewetted materials were soaked in water for 24 h and conditioned for 24, 48, and 72 h. As can be seen, the data for fresh corn show a nearly linear dependence of the drying rate with moisture content which contrasts with those for rewetted particles. Compared with fresh corn, drying of rewetted grains occurs at higher rates, mainly at the higher moisture levels. It is also apparent that although the drying rate of the rewetted material decreases with an increase in the conditioning time, a considerable difference

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0.8 0.7 Moisture (kg water/kg d.b.) 0.6 0.5 0.4 0.3 0.2 0.1 0 0 25 50 75 100 125 Drying time, min 150 175 200

0.5

0.4 Moisture (kg water/kg d.b.)

0.3

0.2

0.1

0 0 25 50 75 100 125 Drying time, min 150 175 200

Fig. 1. Drying curves for fresh and hydrated corn and amaranth grains at 80 1C: (a) (}) fresh corn; () corn grains soaked in water for 48 h and conditioned for 72 h; (m) corn grains hydrated by addition of water and conditioned for 72 h; (K) corn grains hydrated by contact with humid air for 7 days; (b) (}) fresh amaranth; () amaranth grains hydrated by addition of water and conditioned for 24 h; (m) amaranth grains hydrated by contact with humid air for 5 days.

between drying rates for fresh and rewetted grains still exists after a 72 h conditioning period. Moisture in rewetted corn appears to be in a loser state compared to moisture in fresh corn. These differences, however, become smaller as moisture content is reduced until a critical moisture content, below which a relatively small difference is observed. The shape of the curves for fresh and rewetted particles suggest that drying of rewetted particles show the existence of two decreasing drying periods, on the other

hand fresh corn seem to show only one decreasing drying period for the same moisture content range. Fig. 2(b) shows the time variation of moisture content for drying of fresh corn and drying of grains rehydrated by addition of water. The results are similar to those found for corn rewetted by soaking in water (Fig. 2(a)), but at the high moisture content level the drying rates are still larger for grains rewetted by addition of water than those observed for material rewetted by soaking. Fig. 2(c) shows for amaranth grains the time variation of moisture content as a function of moisture content for drying of fresh grains and drying of grains hydrated by addition of water and conditioned for 24 and 72 h. It is clear that drying rates for fresh and rewetted particles seem to follow a common dependence with moisture content and no clear difference seems to occur due to the larger initial moisture content in the rewetted particles. The drying rates of rewetted grains were not affected by an increase in the conditioning time from 24 to 72 h, which suggests that both of them are above the minimum period of time required for moisture to diffuse inside the particle and bond itself to the solid structure in a similar fashion to that observed in fresh amaranth. From the above results, although similar procedures were followed for rewetting both corn and amaranth grains, the drying differences between fresh and hydrated grains seem to be comparatively more evident for corn than for amaranth grains and this would be inuenced by both, the solid nature and particle size. It is expected that the interaction between the moisture content and the solid structure will affect the rate of rehydration, and in terms of a diffusion model such effect can be expressed in terms of the hydration effective diffusion coefcient, where the larger the value of diffusion coefcient the faster the moisture is expected to be absorbed and distributed within the solid. There are experimental works reported in the literature regarding hydration kinetics of corn and amaranth grains, and which either report values for the hydration diffusion coefcient or it can be calculated from the hydration curves. For a Mexican corn similar to that used in this work, Ramos et al. (2004) reported a hydration diffusion coefcient in liquid water (at 313 K) of 3.39 1011 m2/s. For amaranth, Resio, Aguerre, and Suarez (2006) have reported the hydration kinetics in plain water at different temperatures, and from which a hydration diffusion coefcient in liquid water (at 313 K) of 7.36 1012 m2/s has been calculated here based on the solution of Ficks second law. From a comparison between both values it is evident that the diffusion coefcient for corn is more than four times larger than that for amaranth and hence moisture transport can be expected to occur at a faster rate within the former. Furthermore, the difference in particle size will also have an effect on the hydration rate. The resistance to moisture transport is expected to increase with the size of the grain, and since the amaranth and corn particles had an average diameter of 0.9 and 10.6 mm, respectively, transport will be more adversely

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0.012 0.01 0.008 -(dX/dt) -(dXdt) 0.006 0.004 0.002 0 0 0.2 0.4 0.8 0.6 X (kg of water/kg d.b.) 0.04 1

0.012 0.01 0.008 0.006 0.004 0.002 0 0 0.2 0.4 0.6 0.8 X (kg water/kg d.b.) 1

0.03 -(dX/dt)

0.02

0.01

0 0 0.1 0.2 0.3 0.4 X (kg water/kg d.b.) 0.5

Fig. 2. Time variation of moisture content for drying of fresh and hydrated corn and amaranth grains at 80 1C: (a) (&) fresh corn; corn grains hydrated by soaking in water for 24 h and conditioned for: () 24 h; (m) 48 h; (K) 72 h; (b) (}) fresh corn; corn grains hydrated by addition of water and conditioned for: () 24 h; (m) 72 h; (c) (}) fresh amaranth; amaranth grains hydrated by addition of water and conditioned for: () 24 h; (m) 72 h.

affected in corn grains than in amaranth particles. In terms of the characteristic time, p2 R2 =Deff , which corresponds to av the time necessary for the grain to reach 63% of the equilibrium moisture content, it is found that for corn this time is about 30 times larger than that for amaranth. Such signicant difference in the characteristic hydration time seems to explain the need for much larger conditioning times required for corn as compared to amaranth, and this is basically due to the differences in particle size. For similar hydration conditions of both grains, the smaller size of amaranth seems to allow moisture to be absorbed in a closer manner to what is found in the fresh material. Although the differences between hydrated and fresh corn decreases with conditioning time, the latter is found to be limited by the germination of the seed. 3.2. Diffusion coefcient estimation The drying diffusion coefcients were determined from the solution to Ficks second law. The moisture balance equation is given by the second Ficks law that in spherical

coordinates is qX 1 q qX 2 r2 D ; qt r qr qr 0prpR; t40; X e pX pX 0 . (1a)

In drying of spherical particles the boundary and initial conditions are:   qX r0: 0; t40, (1b) qr rR: t0: X R; t X e ; X r; 0 X 0 ; t40, 0prpR. (1c) (1d)

The average concentration inside the particle can be obtained, at each time instant, by the next averaging equation: Z R 3 X r; tr2 dr. (2) X t 3 R 0 Considering the diffusivity independent of the moisture content and equilibrium conditions at the gassolid

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Deff (m2/s)

interface, the solution for a spherical geometry to Ficks equation is (Crank, 1975) "   # 1 6X1 np 2 X Xe exp Dt , (3) Rav X 0 X e p2 i1 n2 where X is the grain average moisture content, X0 is the initial moisture content, Rav is the kernel initial average radius (m), D is the diffusion coefcient (m2/s), t denotes drying time (s), and n is the order of approximation. Xe is the equilibrium moisture content which was determined making use of the correlations reported in the literature (Vizcarra Mendoza, Mart nez Vera, & Caballero Dom nguez, 2003; Zahed & Epstein, 1992). The diffusion coefcients were estimated taking into account only the rst term of the innite Fourier series solution and following a linear regression procedure. In order to take into account the non-sphericity of the grains, the radius of the equivalent sphere was used in the calculations (Kunii & Levenspiel, 1991). As was described in the previous section for corn and amaranth, for the conditions considered in the present work, it was only for corn that an effect was observed of the rehydration process on the drying characteristics of the grain, therefore, the following sections focus only on fresh and rewetted corn grains. The diffusion coefcients have been determined for corn grains for the rst decreasing drying period and the results are presented in Fig. 3. As can be seen from Fig. 3(a), for the grain hydrated by soaking it in water lower diffusion coefcients values were obtained as the conditioning period was increased. However, for all these hydrated materials the diffusion coefcients were larger than the one observed for the fresh grain. This result is in accordance with the higher drying rates observed for the hydrated materials as it is shown in Fig. 2(a). For grains rewetted by addition of water (Fig. 6(b)), the magnitude of the drying diffusion coefcients also decreased with an increase in the conditioning time and was also always larger than that for fresh corn. When compared with moisture in the fresh material, it seems that in the rehydrated materials moisture was in looser state and that the bonding between water and the solid structure can be strengthened by the conditioning time. The diffusion coefcients for fresh and hydrated corn have been obtained for temperatures in the 40100 1C range and their relationship has been correlated in Fig. 4. Following an Arrhenius type of equation (where Deffo corresponds to the effective diffusion coefcient at T0 313 K), and from a linear regression analysis the slopes for the lines for fresh and hydrated grains obtained were 819.2 and 2165.3 K, respectively. It is quite evident from the magnitude of both slopes that moisture transport in hydrated grains was comparatively more sensitive to temperature changes than that in fresh corn grains, and therefore, the diffusion coefcients increases more rapidly with temperature for the hydrated materials. The larger

1.7E-09

1.3E-09 24 h 48 h 9E-10 72 h

5E-10 Fresh corn 1E-10 Grain 2.1E-09 1.7E-09 Deff (m2/s) 1.3E-09 9E-10 5E-10 1E-10 Grain
Fig. 3. Drying effective diffusion coefcients for fresh corn and for grains hydrated by: (a) soaking them in water for 24 h and conditioned for 24, 48, and 72 h; (b) addition of water and conditioned for 24 and 72 h.

24 h

72 h

Fresh corn

0.5 ln (Deff /Deffo) 1 1.5 0 -0.0002 1/T-1/To -0.0004 (K-1) -0.0006

Fig. 4. Effect of temperature on the effective diffusion coefcients for: (~) fresh corn; () hydrated grains by soaking during 48 h in water and with a 72 h conditioning period.

temperature effect on moisture transfer observed for hydrated grains can be explained by weaker moisturesolid interactions as compared to those in fresh grains.

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3.3. First-order kinetic model

1.4

A rst-order irreversible kinetic equation has been employed to predict the drying rates of fresh and rehydrated corn grains. The use of this model has been reported previously for the isothermal drying of materials where internal evaporation is assumed to be the limiting step (Roberts & Tong, 2003). The equation can be written as dX kX X e , (4) dt where X is the grain moisture content during drying (db), k is the rate constant in min1, Xe is the grain equilibrium moisture content (db), and t is the drying time (min). Integration of Eq. (4) yields X Xe MR expkt, X0 Xe (5)

1.2 -ln((X-Xe)/(X0-Xe)) 1 0.8 0.6 0.4 0.2 0 0 20 40 60 Time, min 80 100

2 -ln((X-Xe)/(X0-Xe)) 1.6 1.2 0.8 0.4 0 0 20 40 60 Time, min 80 100

where MR is the moisture ratio, and X0 corresponds to the initial grain moisture content (db). It is interesting to note that this equation corresponds to the following Eq. (6) when in the latter the exponent n is equal to 1: X Xe MR expktn . X0 Xe (6)

This is known as the Page model and it is an empirical expression that it is often used in describing the weight loss versus time data obtained in constant environment for drying and in which k and n are water mobility parameters (Chen, 2006). The grain moisture content as a function of time for different drying temperatures has been plotted in terms of Eq. (5) and it is shown in Fig. 5. The data corresponds to fresh corn and to corn hydrated by soaking in water. For all the drying temperatures, it is clear from this gure that Eq. (5) adequately describes the data for both fresh and hydrated corn grains, and, therefore, from the slopes of each tted line the drying rate constant for each temperature was obtained. As can be seen in Fig. 5, the magnitude of the slopes increases with temperature and hence does the rate constants. Furthermore, at a given temperature, when the slopes for fresh and hydrated grains are compared with each other, it is evident that larger rate constants tend to occur for the rehydrated materials. This result is in accordance with the higher drying rates observed for hydrated corn as compared to those for fresh corn (see Fig. 2(a)). The rate constants obtained from Fig. 5 were assumed to be temperature dependant through an Arrhenius relationship, that is   E a k k0 exp . (7) RT The variation of the drying rate constants with temperature was obtained in terms of Eq. (7) and the results are shown in Fig. 6. From the slopes of the

Fig. 5. Comparison of grain moisture content as a function of drying time with Eq. (3) at different drying temperatures for: (a) fresh corn; and (b) corn hydrated by soaking in water for 48 h and conditioned during 72 h. Temperatures: (~) 40 1C; () 60 1C; (m) 80 1C; (J) 100 1C.

6.5 6 5.5 5 4.5 4 3.5 3 0.0026

-ln(k)

0.0029 1/T (K-1)

0.0031

0.0034

Fig. 6. Arrhenius plot of rate constant versus inverse temperature for: () fresh; (~) hydrated corn.

equations obtained by regression analysis of the data for each grain the activation energies were calculated and found to be 18.6 and 31.2 kJ/mol for hydrated and fresh corn grains, respectively. When compared with that for fresh corn, a smaller activation energy observed for the

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1316 R.S. Ruiz et al. / LWT - Food Science and Technology 41 (2008) 13101316 Campana, L. E., Sempe, M. E., & Filgueira, R. R. (1993). Physical, chemical, and baking properties of wheat dried and microwave energy. Cereal Chemistry, 70(6), 760762. Chen, X. D. (2006). Moisture diffusivity in food and biological materials. In Proceedings of the 15th international drying symposium, Budapest, Hungary. (pp. 1828). Crank, J. (1975). The mathematics of diffusion (2nd ed.). Oxford: Clarendon Press pp. 90103. Devahastin, S., Mujumdar, A. S., & Raghavan, G. S. V. (1998). Diffusioncontrolled batch drying of particles in a novel rotating jet annular spouted bed. Drying Technology, 16(35), 525543. Kunii, D., & Levenspiel, O. (1991). Fluidization engineering (2nd ed.). Boston: Butterworth-Heinemann 61pp. Mart nez-Vera, C., Ruiz-Mart nez, R. S., & Vizcarra-Mendoza, M. G. (2005). Effect of the moistening process on the drying characteristics of grains. In Proceedings of the third inter American drying conference (Paper X-1), Montreal, Canada. Mourad, M., Hemati, M., & Laguerie, C. (1995). Sechage de ma s en lit ` uidise a ottation. I: Etude experimentale de la cinetique de sechage. Chemical Engineering Journal, 59, 221228. Ramos, G., Pezet-Valdez, M., OConnor-Sanchez, A., Placencia, C., & Pless, R. C. (2004). Hydration rates for various types of Mexican maize based on single-kernel measurements. Cereal Chemistry, 8(13), 308313. Resio, A. C., Aguerre, R. J., & Suarez, C. (2006). Hydration kinetics of amaranth grain. Journal of Food Engineering, 72, 247253. Roberts, J. S., & Tong, C. H. (2003). Drying kinetics of hydroscopic porous materials under isothermal conditions and the use of a rstorder reaction kinetic model for predicting drying. International Journal of Food Properties, 6(3), 355367. Tosi, E. A., & Re, E. D. (1999). Amaranth grain drying in a uidized bed. Drying Technology, 17(4/5), 909914. Vizcarra Mendoza, M. G., Mart nez Vera, C., & Caballero Dom nguez, F. V. (2003). Thermal and moisture diffusion properties of amaranth seeds. Biosystems Engineering, 86(4), 441446. Zahed, A. H., & Epstein, N. (1992). Batch and continuous spouted bed drying of cereal grains: The thermal equilibrium model. Canadian Journal of Chemical Engineering, 70, 945952.

hydrated corn signify that less energy was required to remove the moisture from the hydrated kernels, and, therefore, it could be said that moisture in the employed hydrated grains appears to be in a looser state than moisture in the fresh material. 4. Conclusions Corn kernels rewetted by different methods have been found to show higher drying rates than the fresh material when dried under equivalent conditions. When compared with moisture in the fresh material, it seems that moisture in the hydrated materials was in a looser state and that the bonding between water and the solid structure can be strengthened by the conditioning time. This result was more evident as the drying temperature was increased. In accordance with these ndings larger effective diffusion coefcients were obtained for the hydrated corn as compared with those for the fresh grains. Furthermore, when a rst-order kinetic model was employed, smaller activation energies were obtained for the hydrated materials, which suggests that less energy is required to remove moisture from these solids. Rewetted amaranth, on the other hand, was found to show similar drying rates to those obtained with fresh grains. Amaranth grains are about an order of magnitude smaller than corn grains, therefore, it appears that the grain size, as part of the moisture diffusion resistance in the rewetting process, is a key factor that determines the time required for the moisture to be absorbed and distributed uniformly when trying to reproduce the drying behavior of fresh grains. References
Beke, J., Mujumdar, A. S., & Bosisio, R. G. (1995). Drying of fresh and rewetted shelled corn in microwave elds. Drying Technology, 13(1/2), 463475.