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Superheated Steam Drying of Distillers' Spent Grains on a Single Inert Particle

Magdalena Zielinska a; Stefan Cenkowski b; Marek Markowski a a Department of Agri-Food Process Engineering, University of Warmia and Mazury, Olsztyn, Poland b Department of Biosystems Engineering, University of Manitoba, Winnipeg, MB, Canada Online publication date: 04 December 2009

To cite this Article Zielinska, Magdalena, Cenkowski, Stefan and Markowski, Marek(2009) 'Superheated Steam Drying of

Distillers' Spent Grains on a Single Inert Particle', Drying Technology, 27: 12, 1279 1285 To link to this Article: DOI: 10.1080/07373930903195065 URL: http://dx.doi.org/10.1080/07373930903195065

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Drying Technology, 27: 12791285, 2009 Copyright # 2009 Taylor & Francis Group, LLC ISSN: 0737-3937 print=1532-2300 online DOI: 10.1080/07373930903195065

Superheated Steam Drying of Distillers Spent Grains on a Single Inert Particle

Magdalena Zielinska,1 Stefan Cenkowski,2 and Marek Markowski1
1 2

Department of Agri-Food Process Engineering, University of Warmia and Mazury, Olsztyn, Poland Department of Biosystems Engineering, University of Manitoba, Winnipeg, MB, Canada

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The article presents the results of drying a distillers spent grain fraction (DSG) of a stillage in superheated steam (SS). The study aimed at determination of the effect of SS parameters on drying kinetics of DSG deposited as a pasty layer on the 50-mm solid Teon sphere. Drying was conducted at approximately 2 to 4 kPa above the atmospheric pressure, with steam temperature ranging from 110 to 160 C and steam velocity of 1 m/s. Samples were dried with SS at different processing times ranging from 60 to 360 min, depending on the SS temperature. During the initial warmup period of SS processing, the pasty DSG gained moisture due to steam condensation on its surface, which further evaporated at constant material temperature (apparent constant rate period). That period ended as soon as the condensate evaporated and temperature of the product passed the saturation point of steam. Only the falling drying rate period was observed. The drying rates increased from 0.02 to 0.83 L/min with the increase in steam temperature from 110 to 160 C, respectively. The effective diffusivity of moisture in DSG increased with the increase in steam temperature according to the Arrhenius-type relationship. The values of the effective diffusivity ranged between 3.24 1010 and 2.48 109 m2/s, with the activation energy of 53.74 kJ/mol. Keywords Distillers spent grain; Drying; Single inert particle; Stillage; Superheated steam

INTRODUCTION Distillers spent grain (DSG) is the by-product of ethanol production left in distilleries after fermentation. Possible grains used in fermentation are corn, wheat, barley, rice, and rye.[1,2] DSG is an excellent source of protein and energy and is mainly used as feed for animals, but it can also be used as a supplement to produce food for human consumption; e.g., extruded snacks and baby food products.[3] Alcohol production concentrates the proteins, fat, and bers from the grain in DSG. If the grain is contaminated, the drawback is a concentration of any toxins from fungal growth, including mycotoxins from Fusarium
Correspondence: Magdalena Zielinska, Department of AgriFood Process Engineering, University of Warmia and Mazury, Heweliusza 14, 10-718 Olsztyn, Poland; or Department of Biosystems Engineering, University of Manitoba, Winnipeg, MB, Canada R3T 5V6; E-mail: m.zielinska@uwm.edu.pl

species, such as deoxynivalenol (DON), a trichothecene mycotoxin produced by Fusarium graminearum.[4] To prolong the storage time and lower the transportation cost, DSG needs to be dried to about 10% w.b. (wet basis) moisture content.[2] Typical drying operations that use hot air are energy intensive. To save energy, hot air could be replaced by superheated steam (SS) as the drying medium. In addition, SS drying has some other advantages over the air drying, including the reduction in the environmental impact, an improvement in drying efciency, the elimination of re or explosion risk, and a recovery of valuable volatile organic compounds.[3] Superheated steam dryers have been used to dry a number of food products on the pilot, laboratory, and industrial scale, including green tea, sugar beet pulp, potato chips, vegetables, noodles, herbs, and spices.[47] Drying in SS is of interest to distillers because current techniques using hot air as a drying medium are not capable of eliminating mycotoxins or reducing them to a level that is low enough in DSG that it can be sold to livestock producers as feed.[8] The objective of this study was to determine the effect of SS on drying kinetics of distillers spent grain dried on an inert Teon sphere. MATERIAL AND METHODS Material The work was carried out using stillage obtained from a distillery (Mohawk Canada Limited, a division of Husky Oil Limited) in Minnedosa, Manitoba, processing wheat into ethanol. A laboratory centrifuge (Sorvall General Purpose, RC3, Thermo Scientic Co., Asheville, NC) was used to separate the stillage into three fractions: solid DSG, paste, and liquid. The relative centrifugal force was 790 g, with a sample container rotating speed of 2200 rpm on the radius of 0.146 m. Stillage was centrifuged in a 1000-mL container for 10 min. Only fraction of the highest density (solid DSG) was used in the SS drying experiments. The initial moisture content of that fraction was 77.2 0.8% w.b. Moisture content was determined by the air-oven drying method according to the AACC standards.[9] The solid DSG

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fraction was stored in a deep freezer at 15 C and thawed at room temperature when needed in a drying experiment. DSG was dried on a solid Teon sphere (150 g; 5.0 cm in diameter) that served as the inert material. The inert material was used to develop surface area for a better interaction between superheated steam and DSG. Each sample needed for one drying experiment weighed approximately 22 1 g. A layer (approximately 3 mm thick) of wet DSG was uniformly distributed on the surface of a Teon sphere using two hemispherical tea strainers with approximately 3 mm radius greater than the radius of the inert material. Drying Experiment Steam Dryer The fundamental drying experiments were carried out in an SS dryer designed and fabricated in the Department of Biosystems Engineering, University of Manitoba (Fig. 1). The system comprised a steam generator (1), a superheater (6), steam-conveying pipes and valves (5, 8, 12, 14, 16, 22), a drying chamber (13), a process water tank (17), a condensation unit (23), a data acquisition, and a control system (not shown in Fig. 1). The drying system was fully described in the literature.[8] An electric boiler (ES18, Sussman-Automatic Corp., Long Island City, NY) generated saturated steam at a pressure of approximately 10 bars. The saturated steam was then heated by the 4-kW Caloritech superheater (Sussman Electric Boilers, Long Island City, NY). The various valves placed throughout

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the system controlled the steam path and ow velocity. The superheated steam unit was designed with a steam bypass that diverted the steam from the drying chamber during the warmup and sample loading periods. To facilitate that bypass, a three-way automatically controlled solenoid valve (12) was installed. A cubical drying chamber (224 224 mm cross section) was separated by a metal plate (11) into two sections: upper (1) and lower (2), with the aim of creating uniform SS velocity prole inside the upper chamber (Fig. 2). The design intent was for the superheated steam to ll the lower chamber and be uniformly funneled through a 210-mmlong and 89-mm-diameter stainless steel pipe (4) that connected these two sections. A Teon sphere (7) with a sample (8) was suspended by a string (5) from an electronic balance (9). To maintain the same drying conditions (SS temperature and velocity) around a sample, a ring xture (3) was placed around the sample. During drying, the outer surface of the chamber was heated by electric strip heaters, ensuring that the chamber walls were at the same temperature as the superheated steam. This solution created adiabatic conditions for the chamber and the drying sample, preventing any possible condensation of steam on the walls. Processing Conditions Experiments were carried out under different SS temperatures of 110, 130, 140, 150, and 160 C and steam velocity of 1 m=s. Drying was carried out at a chamber

FIG. 1. Schematic diagram of the superheated steam processing system: 1: steam generator; 2: globe valve; 3: steam trap; 4: vacuum breaker; 5: pressure-reducing valve; 6: superheater; 7: pressure gauge; 8: steam relief valve; 9: vortex meter; 10: pressure transducer; 11: thermoelectric probe; 12: three-way solenoid valve; 13: drying chamber; 14: steam relief valve; 15: pressure gauge; 16: check valve; 17: process water tank; 18: sparge tube; 19: pump; 20: valve; 21: pressure gauge; 22: ball valve; 23: condensation unit.[15]

FIG. 2. The superheated steam drying chamber: 1: upper drying chamber; 2: lower drying chamber; 3: ring xture; 4: stainless steel pipe; 5: string; 6: berglass mesh; 7: Teon sphere; 8: DSG sample; 9: balance; 10: fan; 11: steel plate.

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pressure of 102104 kPa. The drying chamber was heated up for 1 h before an experiment. This was needed to bring the temperature of the chamber above the saturation point to avoid possible steam condensation on the inner walls. Samples were dried with SS at different processing times, ranging from 60 to 360 min depending on the SS temperature. All samples were dried to the same nal moisture content of 6.8 2.0% w.b. Mass and temperature changes of DSG dried in SS were measured in separate experiments conducted under the same conditions. Under each set of drying conditions, the drying tests were conducted in triplicate. An arithmetic average was then taken for data interpretation. Superheated Steam Flow Measurement Steam velocity was calculated from the readings displayed by the computerized mass ow rate meter (Compart DXF 351 Flow Computer, Endress Hauser GmbH Co., Weil am Rein, Germany). The specic volume of SS for selected conditions was determined from SS tables.[10] The steam ow rate and its velocity were adjusted by the steam relief valve (No. 8 in Fig. 1). Temperature Change Measurement The temperature at various locations inside the drying chamber was measured with 30-gauge K-type thermocouples connected to a data acquisition system. Four K-type thermocouples were required to measure the temperature inside the chamber. These thermocouples were located along the height of the lower and the upper chambers. Furthermore, three thermocouples were inserted into a sample to measure the temperature in the center of the Teon sphere and its surface and to measure the temperature of the dried material by embedding the thermocouple tip into the DSG layer by 1.5 mm. The temperature changes were recorded every 3 s by a computer with an accuracy of 1 C. Pressure Measurement Adequate monitoring of the pressure in the SS system was performed by three pressure gauges: two for the superheated steam (No. 7 and No. 15 in Fig. 1) and one for the water in the boiler (No. 21 in Fig. 1). The accuracy of the measurements was 0.1 kPa. Mass Change Measurement Separate drying experiments were performed to measure the mass changes of samples during drying (Fig. 2). The Teon sphere (7) covered with DSG (8) was attached to a string (5) and suspended from a digital electronic scale (9) positioned on top of the upper chamber (1). A cooling fan (10) was installed between the chamber and mass balance (9) to prevent any rise in temperature of the platform scale due to steam leaking from the small orice in

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the inner chamber, causing the balance to wet and=or overheat (Fig. 2). To prohibit high-moisture DSG from dripping off the sphere, an outside berglass mesh-cage (6) was used around the sphere. The specic properties of berglass (high heat resistance and low hygroscopicity) were taken into consideration when choosing a material that would not soften and melt or absorb moisture in the presence of SS. Changes in moisture content of a sample were calculated based on the measured mass changes, which were recorded with an accuracy of 0.001 g using an electronic balance (Model TR-403, Denver Instrument Co., Arvada, CO). The mass balance was connected to a computer and the samples changes were recorded every 3 s. The drying was stopped when the mass of the sample remained constant for 5 min. Calibration Test During drying, the upward ow of superheated steam through the drying chamber created a lifting force, dened as the measured mass readings with and without steam passing through the drying chamber, that inuenced the real mass measurements. This lifting force was taken into the calculation of the real mass changes during drying. To account for the lifting force, separate experiments were conducted after each drying experiment. The steam conditions were kept the same as during the drying tests. The SS ow was manually controlled to bypass the inner drying chamber every 2 min for 2 min. Each time the solenoid valve was engaged, the pressure in the drying chamber increased slightly by approximately 2 kPa and then returned to its original (previous) pressure. The short-term change in pressure and steam velocity at the beginning of each interruption in the calibration test had a tendency to change the lifting force and affected the mass measurements. Therefore, the pressure increase at the beginning of each calibration measurement was not taken into calculation. The exemplied measurement for mass changes with and without steam passing through the drying chamber during DSG drying in superheated steam at 160 C is shown in Fig. 3. The overall difference between the measured mass readings with and without steam passing through the drying chamber for all drying conditions was about 1 g. Moisture Diffusion Analysis It was assumed that the conditions of moisture transfer in the thin layer (3 mm) of DSG dried on inert material were similar to those observed for an innite plate dried from one side by the constant steam ow and temperature, whereas the other side of the plate was water impermeable. The effective diffusivity of moisture can be calculated in analogy with the analytical solution of one-dimensional Ficks law of diffusion with constant moisture diffusivity

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models were determined using a nonlinear regression procedure based on the Levenberg-Marquardt algorithm. The concordance between experimental and calculated data was determined using the coefcient of determination (R2). RESULTS AND DISCUSSION Drying Kinetics Temperature Change Measurements Figure 4 shows a representative temperature history of the thin layer of DSG dried on the inert material. The diagram shows three lines, each corresponding to a different location of the thermocouple tip (surface and center of the inert material and DSG temperature). The experiments were conducted at SS temperature of 130 C. Initially, the heat supplied to the material was used to increase the materials temperature. Therefore, a typical short warmup period was observed until the temperature of the product reached 100 C (saturation temperature). Then, a period of constant temperature of 100 C occurred. This period was associated with the evaporation of the condensate (free water) from the surface of a sample and could be mistakenly interpreted as the rst drying rate period because the temperature of the product was constant due to steam condensation. Both the duration of the warmup period and the constant temperature period were related to the SS temperature. The duration of the warmup and the constant temperature periods ranged from 2 to 10 min and from 20 to 80 min, respectively. In the nal period, a typical SS drying curve shows a slow increase in materials temperature, which eventually reaches the SS temperature. This happens when the equilibrium moisture content between the product and the SS is reached and is in agreement with the data reported by other researchers.[6,7,12]

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FIG. 3. Mass changes due to the lifting force for DSG dried on the inert material in SS at 160 C.

and when the shrinkage phenomenon is assumed negligible. This problem can be mathematically expressed in the following form: " !# 1 X Xe 8 X 1 p2 2n 12 Fom exp X0 Xe p2 n0 2n 12 4 1 The Fourier number for mass transfer is Fom De t s2 2

Generally, s represents a half of the plate thickness if the innite plate is suspended in the drying medium and moisture is transferred from both sides of the plate. In our particular case, moisture was removed from one side; namely, from the outer layer. Therefore, the parameter s represents here the whole thickness of DSG layer on the inert material. The effective diffusivity (De) can be calculated from the following empirically found drying constant (K):[11] K p2 De 4s2 3

Temperature dependence of the effective moisture diffusivity coefcients follows the Arrhenius-type equation:[11]   Ea De D0 exp 4 RT 273:15 Statistical Analysis Data were analyzed using the software package Statistica 7.0 (StatSoft Inc., Krakow, Poland). The constants of

FIG. 4. Typical temperature characteristics of DSG dried on inert material (5-cm-diameter Teon sphere) in SS at 130 C (dashed line indicates steam temperature).

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Mass Changes Measurements The changes in moisture content over drying time are shown in Fig. 5. During the warmup period, the DSG samples gained moisture due to steam condensation on the material surface as long as the sample temperature was below the saturation point for steam (100 C). The insert in Fig. 5 shows the enlarged initial stage of processing in SS. The DSG samples gained more moisture during processing at lower SS temperatures. The higher SS temperatures allowed faster removal of the condensate. Thereafter, when a period of constant temperature at 100 C occurred, the heat supplied to the material was used only to vaporize the free water that condensed on the material surface. This period resembled the constant drying rate but was not associated with it. The moment at which the slow increase of material temperature was observed indicated the beginning of the moisture removal stored in the sample and the moment when the condensate evaporated so the moisture content of the sample attained its initial value. This last period resembled the falling drying rate period. The drying times for reaching the equilibrium moisture content were 360, 160, 120, 80, and 60 min for the SS temperatures of 110, 130, 140, 150, and 160 C, respectively. The increase in steam temperature from 110 to 160 C resulted in shortening drying time by 83% (Fig. 5). Experimental results of moisture variation with drying time were tted to the theoretical model (Eq. (1)). Only the rst 11 terms in the series solution (Eq. (1)) were considered because the higher number of terms in the series did not improve the model accuracy. The total time of steam condensation on the surface of a dried material

was not taken into consideration during modeling the drying kinetics. Therefore, only the data limited to the period of material drying were tted to the theoretical model. In all cases, the values of R2 greater than 0.9 indicated a good t.[13] It was concluded that Eq. (1) is a useful theoretical model for correlating moisture content with time during drying. Drying Rates Calculation Mathematical differentiation of the drying curves shown in Fig. 5 (not including warmup period and condensation and evaporation of the condensate) allowed the calculation of the drying rates.[14] The drying rate vs. moisture content is shown in Fig. 6. The curves begin after the condensate evaporated from the surface and samples regained their original moisture content. No constant drying rate period was observed for any experiments performed. The higher the SS temperature, the greater the increase in drying rates that was observed. During the initial phase of SS drying the drying rates of DSG increased with increasing temperature; i.e., 0.02, 0.25, 0.31, 0.49, and 0.83 L=min for steam temperatures of 110, 130, 140, 150, and 160 C, respectively (Fig. 6). Determination of the Effective Diffusivity (De) and Energy of Activation (Ea) The values of the effective diffusivity calculated from Eq. (3) ranged from 3.24 1010 to 2.48 109 m2=s. According to the Arrhenius-type equation, the effective moisture diffusivity coefcients reported in this study were correlated with the reciprocal of the drying medium temperature. In reality, however, the effective moisture diffusivity depends on material temperature. Therefore, this

FIG. 5. Moisture changes in DSG during drying in SS at 110, 130, 140, 150, and 160 C. The insert shows the enlarged initial stage of processing in superheated steam.

FIG. 6. Changes in the drying rates of DSG dried in SS at 110, 130, 140, 150, and 160 C.

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approach is correct assuming that the average material temperature is not that different from the steam temperature. The correlation between the effective diffusivity of moisture in DSG and the inversed medium SS temperature is shown in Fig. 7. The variation in the effective diffusivity at 110, 130, 140, 150, and 160 C was observed to be linearly correlated with the reciprocal of the drying medium temperature (R2 > 0.9703). The activation energy of 53.74 kJ=mol was determined by linearizing the effective moisture diffusivity against temperature (Fig. 7). CONCLUSIONS From this exploratory study on the particularities of drying DSG in SS the following conclusions can be drawn:
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4. The effective diffusivity (De) of moisture in DSG increased with the increase in SS temperature according to the Arrhenius-type relationship. The values of the De ranged from 3.24 1010 to 2.48 109 m2=s, and the activation energy (Ea) was equal to 53.74 kJ=mol. NOMENCLATURE Effective moisture diffusivity (m2=s) De D0 Constant in Eq. (4) (m2=s) Ea Activation energy for moisture diffusion (kJ=mol) Fom Fourier number K Drying constant (1=s) R Gas constant (R 8.314 kJ=mol K) s Thickness of DSG layer on the Teon sphere (m) T Steam temperature ( C, K) t Drying time (min) X Actual moisture content (kg water=kg d.b.) Xe Equilibrium moisture content (kg water=kg d.b.) X0 Initial moisture content (kg water=kg d.b.) ACKNOWLEDGMENT The study was nancially supported by the Polish Ministry of Science and Higher Education through the program entitled Supporting International Mobility of Researchers and by the Natural Sciences and Engineering Research Council of Canada. REFERENCES
1. Wampler, D.J.; Gould, W.A. Utilization of distillers spent grain in extrusion processed doughs. Journal of Food Science 1984, 49 (5), 13211322. 2. Woods, B.; Husain, H.; Mujumdar, A.S. Techno-Economic Assessment of Potential Superheated Steam Drying Applications in Canada; Canadian Electrical Association: Montreal, QC, Canada, 1994. Report 9138 U 888. 3. Tang, Z.; Cenkowski, S.; Izydorczyk, M. Thin-layer drying of spent grains in superheated steam. Journal of Food Engineering 2005, 67, 457465. 4. Urbaniec, K.; Malczewski, J. Experimental investigations of beet pulp drying in superheated steam under pressure. Drying Technology 1997, 15 (6&8), 20052013. 5. Tang, Z.; Cenkowski, S. Comparison of the dehydration dynamics of potatoes in superheated steam and hot air. Canadian Agricultural Engineering 2000, 42 (1), 4349. 6. Markowski, M.; Cenkowski, S.; Hatcher, D.W.; Dexter, J.E.; Edwards, N.N. The effect of superheated-steam dehydration kinetics on textural properties of Asian noodles. Transaction of ASAE 2003, 46 (2), 389395. 7. Pronyk, C.; Cenkowski, S.; Muir, W.E. Drying foodstuffs with superheated steam. Drying Technology 2004, 22, 899916. 8. Cenkowski, S.; Pronyk, C.; Zmidzinska, D.; Muir, W.E. Decontamination of food products with superheated steam. Journal of Food Engineering 2007, 83, 6875. 9. AACC. Air-oven method, drying at 135 C. In Approved Methods of the American Association of Cereal Chemists: AACC, 10th ed., Method 4415A, St. Paul, MN, 2000. 10. Irvine, Jr., T.F.; Liley, P.E. Steam and Gas Tables with Computer Equations; Academic Press: Orlando, FL, 1984.

1. During the warmup period, the samples gained moisture due to steam condensation on the material surface as long as the sample temperature was below the saturation point for steam (100 C). When a period of constant temperature at 100 C occurred, the heat supplied to the material was used to vaporize the condensed free water from the material surface. In spite of a constant materials temperature, this period should not be confused with a constant drying rate period. Finally, when the slow increase of the materials temperature was observed, the material began to lose its original moisture. 2. When drying in superheated steam, Ficks law of diffusion can be utilized for correlating moisture content with drying time. 3. The drying rate of DSG varied with SS temperature. The higher the SS temperature, the greater the increases in the drying rates that were observed. During the initial phase of SS drying the drying rates of DSG increased with increasing temperature; i.e., 0.02, 0.25, 0.31, 0.49, and 0.83 L=min for steam temperatures of 110, 130, 140, 150, and 160 C, respectively.

FIG. 7. Temperature dependence of the effective diffusivity coefcient.

SUPERHEATED STEAM DRYING 11. Zielinska, M.; Markowski, M. Drying behavior of carrots dried in a spout-uidized bed dryer. Drying Technology 2007, 25, 261270. 12. Tang, Z.; Cenkowski, S.; Muir, W. E. Dehydration of sugar beet pulp in superheated steam and hot air. Transactions of the ASAE 2000, 43 (3), 685689. 13. Kingsly, R.P.; Goyal, R.K.; Manikantan, M.R.; Ilyas, S.M. Effects of pre-treatment and drying air temperature on drying behaviour of

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peach slice. International Journal of Food Science and Technology 2007, 42, 6569. 14. Pabis, S.; Jayas, D.S.; Cenkowski, S. Grain Drying. Theory and Practice; John Wiley and Sons: New York, 1998. 15. Gervais, M.; Pronyk, C.; Bunn, J.; Cenkowski, S. Design and Performance of a Laboratory Scale Superheated Steam Processing System; Paper presented at the North Central ASAE=CSAE Conference, 2425 September, Winnipeg, MB, Canada, 2004.

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