Simultaneous Drying and Modification of Properties of Starch Using Vacuum Microwave Treatment

The prospect of modifying starch properties while drying was investigated. Potato starch (18% moisture, dry basis) was vacuum microwave treated for different durations (60 to 600 s) with power ratings of 600, 1,000, and 1,500 W at a reduced pressure of 5,000 Pa (absolute). The drying rate was observed to be partially constant but was accompanied by a curious rise in sample temperature. Under a polarized light microscope, reduction in granule size was noticed, which was confirmed from the bulk density measurements, and this shrinkage may be explained by the loss of constituent water. Water absorption capacity of the treated starch samples was further studied at 55°C. The results showed a sudden increase in the capacity, indicating a reduction in gelatinization temperature of starch. This may be attributed to the change in nature of starch from crystalline to amorphous as shown by X-ray diffractograms and to the cracks developed on the granule surface during treatment seen in the scanning electron microscope images. This modified starch can serve well in the paper and food industry.     

Energy Consumption during Vacuum Microwave Treatment of Potato Starch: A Phenomenological Model

It is known that the water binding capacity of starch increases after vacuum microwave treatment. Microwave radiation absorbed by the starch sample affects its sensible, latent internal and chemical (bond and conformational) energy levels. A phenomenological model was developed based on energy sinks in starch, practically described as increasing temperature, breaking bonds between water and amylopectin/amylose molecules, changing the phase of water from liquid to vapor and structural rearrangements at short (single/double helices) and long (crystalline/amorphous) order. The model was validated by experimental data for different vacuum microwave treatment parameters, viz. incident power (460, 500 and 750 W), duration (30 to 340 s) and sample mass (10 to 70 g) at 4000 Pa. The results provide an insight into the physical aspects of the process and would facilitate its development on an industrial scale.     

Effect of absorbed power and dopant content on densification during rapid microwave sintering of Bi2O3-doped ZnO

ZnO samples with an addition of 0, 0.035, 0.1, and 0.35 mol.% Bi₂O₃ were microwave sintered at heating rates 10 and 50°C/min to a maximum temperature of 1200°C with zero hold time. The densification curves obtained by optical dilatometry have been studied in their dependence on the dopant concentration and the heating rate. Direct volumetric absorption of microwave radiation resulted in a 50–60°C shift of the densification curves toward low temperatures compared to susceptor-assisted heating. An analysis of the effect of the volumetrically absorbed microwave power on the formation of grain-boundary phases that facilitate densification is presented.     

Effect of propylation on the characteristics of corn starch and variation of properties with different degrees of substitution

Corn starch was modified by propylation with different degree of substitution (DS). DS of four starch modifications were 0.61, 1.56, 2.27, and 2.51. Samples were characterized by FTIR, XRD, TG‐DTA, swelling power, solubility, water binding capacity, and light transmittance. Results of the systematic physico‐chemical characterization of the starch modification in comparison with the native starch have been documented in the article. Results showed that during propylation, the crystalline structure of starch got destroyed and surface of the starch was eroded. Propylated starch (DS 2.51) showed 85% weight loss at temperatures from 300 to 400°C, whereas the native starch underwent similar weight loss (83%) from 250 to 300°C. Swelling power and water binding capacity of native starch (DS 0.0) were 3.09 g/g and 89.8%, respectively. However, in propylated starch at low DS (DS 0.61), swelling power and water binding capacity increased to 10.55 g/g and 136.8% under same conditions. At high DS (DS 2.51), swelling power was similar to native starch at 65°C, whereas solubility and water binding capacity decreased to below that of native starch. Light transmittance of propylated starch with high DS (DS 2.51) increased dramatically compared with native starch. Propylation improved the hydrophobic transformation and thermal stability of starch at high DS. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Influence of treatment temperature on wettability of Norway spruce thermally modified in vacuum

Wettability of Norway spruce modified by a new vacuum thermal modification procedure was studied. The mass loss caused by this process ranged from almost 0% when treated at 140?°C to 4.3% at 210?°C. Apparent contact angles of water, formamide, and diiodomethane were measured by the Wilhelmy plate method on the specimens taken from the centers of the thermally modified wood samples. For the treatment at the highest temperature, the contact angle of water was significantly higher when compared to untreated spruce (96.6° vs. 83.6°); lower treatment temperatures, however, did not result in a clear correlation between treatment temperature and contact angle. Formamide yielded lower contact angles for treated spruce compared to the untreated one, but without clear influence of the treatment temperature and diiodomethane always gave perfect wetting. Surface energy calculations according to the Owens, Wendt, Rabel, and Kaelble method revealed that the thermal modification process in vacuum increased the surface free energy and lowered the polarity of wood significantly only at the highest applied temperature (210?°C); the treatment had only limited effect at lower temperatures of modification. These results indicate that adequate wetting and adhesion can be achieved on the surfaces of Norway spruce thermally modified in vacuum.     

Studies on chemically modified cotton. V. Effect of zinc chloride solutions on swelling and other properties of cotton

This paper describes the effect of zinc chloride solutions of different molarity at different temperatures, viz., 10°, 25°, 36°, 55°, and 75°C, on various properties of cotton fiber such as degree of swelling, accessibility to water vapor and iodine absorption, infrared ratio, barium activity number (BAN), and leveling-off degree of polymerization (LODP). Zinc chloride solution caused inter- and intrafibrillar swelling in cotton fiber depending on conditions of treatment, viz., concentration of solution and temperature employed. Fibers treated in 10.07 moles/1. (M) solution of zinc chloride in slack state showed rapid increase in degree of swelling up to 2 hr, followed by a slow increase, reaching the maximum after 3 hr of treatment. Fibers swollen with fixed ends without allowing shrinkage showed gradual increase with maximum swelling after 6 hr of treatment. Cotton fibers treated in different molar solutions of zinc chloride at 55°C showed varying degrees of swelling (inter- and intrafibrillar) and a somewhat different trend compared to that observed at 10°C. Electron micrographs revealed mostly intercrystalline swelling in case of samples treated with 9.26M at 10°C, while the same concentration produced intracrystalline swelling at 55°C. Accessibility to water vapor, iodine absorption, and BAN of treated samples showed specific effect of temperature with regard to effectiveness of concentrations of zinc chloride solutions. Similar effects of temperature with regard to concentrations of reagent were observed on infrared ratio and LODP. Accessibility by iodine absorption and LODP correlate with BAN; also, the accessibility by iodine absorption correlates with the LODP.     

Effects of hydrothermal ageing on the thermal behaviour of poly(vinyl chloride) filled with wood flour

The hydrothermal ageing of wood‐flour‐filled PVC produced by dry‐blending in a high‐speed mixer in the presence of a plasticizer and other processing additives was carried out to investigate its thermal behaviour, and the results obtained were compared with those for the unfilled material. The dry‐blended compounds were prepared as films by a calendering process. The accelerated hydrothermal ageing was carried out by immersing the samples in boiling water at 100 °C for 110 h. The thermal behaviour of the reference and the aged samples in water was characterized by differential scanning calorimetry (DSC) and determination of the weight changes. The study has shown that during hydrothermal ageing, the samples from the whole formulations absorbed water, for instance, for 30 wt% filled PVC (F30), 16 wt% of water absorption was obtained, while this was only 2.2 wt% for unfilled PVC (F0). It was also noticed that the formulations filled with wood flour up to 10 wt% exhibited similar water absorption kinetics, i.e. the water was mostly absorbed during the first 50 h and the amount absorbed was less than 5 wt%. On the other hand, the 30 wt% filled samples regularly absorbed water up to almost 16 wt% after 100 h of immersion. The DSC data showed that hydrothermal ageing significantly affected the onset temperature of decomposition (T_d) of the unfilled samples by decreasing this temperature from 228 to 215 °C. For the 30 wt% filled samples, only additive migration was observed, while the T_d remained almost unchanged. Furthermore, from the DSC data, processability of the 30 wt% filled PVC samples at elevated temperatures, i.e. 180 to 200 °C was shown. Copyright © 2004 Society of Chemical Industry     

Sorption Properties of Vacuum-Dried Strawberries

This work demonstrates the influence of changes in parameters of vacuum drying (temperature and pressure) on the sorption properties of dried strawberries. Fruits were dried at 50 and 70°C under pressures of 4 and 16 kPa. Vacuum drying was also conducted during the first 4 h at 70°C and then the temperature was decreased to 50°C at a pressure of 4 kPa. The other combination included increasing the pressure after the first 4 h from 4 to 16 kPa at a drying temperature of 70°C. Sorption isotherms were determined in the dried strawberries. It was shown that with increasing drying temperatures, there was a notable deterioration in the capacity for absorbing water vapor by the vacuum-dried fruit. On the other hand, the pressure at which vacuum drying proceeded did not significantly affect water vapor absorption. Changing the parameters of vacuum drying—that is, temperature in the range of 50–70°C and pressure in the range of 4–16 kPa—affected the shape and structure of the resultant dried strawberries. The combination of vacuum drying with convective drying also influenced the shape and structure of the dried fruit.     

Rapid microwave sintering of zinc oxide-based varistor ceramics

Samples of ZnO + Bi₂O₃ + Sb₂O₃ varistor ceramics were microwave sintered using gyrotron systems operating at a frequency of 24 GHz. The microwave power was automatically regulated to implement heating at a constant heating rate of 10–130 °C/min up to a temperature of 1100–1300 °C with no isothermal hold. The final sintered density of the samples was 95–96 % of the theoretical value. Manifestations of the thermal instability associated with the liquid phase formation were observed at a temperature of about 600 °C. The estimated volumetrically absorbed power density at the onset of instability was ≥20 W/cm³, and the temperature difference measured between the center and periphery of the samples reached 200 °C. Correlation has been revealed between the thermal instability occurrence and the shift of densification curves towards lower temperatures. A mechanism underlying enhanced densification in electromagnetic field-assisted sintering processes is suggested.     

Ultra-rapid microwave sintering of pure and Y2O3-doped MgAl2O4

MgAl₂O₄ samples were microwave sintered to near-full density in rapid processes with heating rates on the order of 100°C/min and zero isothermal hold. The experiments were carried out using a gyrotron system for microwave processing of materials operating at a frequency of 24 GHz with a maximum power of 6 kW. In the regimes with a preset heating rate sustained by the automatically regulated microwave power, the maximum achieved density was about 95% of the theoretical value in pristine MgAl₂O₄ samples (maximum sintering temperature 1650°C) and about 97% in 1 wt.% Y₂O₃-doped samples (1700°C). In the regimes with a fixed microwave power (about 3.5 kW), translucent spinel samples with a relative density above 99% were obtained at 1700°C. The duration of the high-temperature stage of sintering was 1.5-10 minutes. The suggested mechanism responsible for the enhanced densification involves development of a thermal instability and formation of transient liquid phases at grain boundaries. The estimated specific absorbed power in the samples during the high-temperature stage of ultra-rapid microwave sintering was 27-80 W/cm³, similar to the values observed in dc field-assisted flash sintering experiments.     

Bridged polysilsesquioxane-derived SiOCN ceramic aerogels for microwave absorption

The development of high-performance microwave absorption materials in harsh environment is highly desirable but challenging. Herein, lightweight silicon oxycarbonitride (SiOCN) ceramic aerogels were fabricated by the pyrolysis of bridged polysilsesquioxane aerogels, which was presynthesized by a sol–gel method followed by vacuum drying. The structural order and content of free carbon phase determined by pyrolysis temperature play a critical role in modulating the impedance matching and attenuation capacity. The as-prepared SiOCN aerogel pyrolyzed at 1000°C achieves a minimal reflection loss of −64.2 dB at 8.96 GHz and a broad bandwidth of 5.4 GHz at a low thickness of 2.15 mm. The hierarchical pore structure, abundant heterogeneous amorphous SiOCN/free carbon interfaces, and conductive free carbon phase benefit the superior absorption performance by forming good impedance matching, multiple scattering, interface polarization, and conduction losses. This work provides an insight for the rational design of polymer-derived ceramic aerogel-based microwave absorption materials for potential application under extreme conditions such as high-temperature and oxidation environments.     

Microwave vs conventional porcelain firing: Macroscopic properties

This paper provides an overview of the macroscopic properties of porcelain tableware fired in a microwave furnace with six magnetrons (each with a nominal power of 900 W) operating at the frequency of 2.45 GHz. The dependence of firing temperature on physical properties such as shrinkage, water absorption, apparent porosity, bulk density, and impact resistance was analyzed. Emphasis is on the differences in the macroscopic properties of microwave and conventionally (gas and electric) fired porcelain. Batches were fired from room temperature up to above the optimum firing temperature (1380°C). Results show similar macroscopic properties for both firing methods, microwave heating required lower firing temperatures (between 1300°C and 1350°C), and shorter processing times (about 70 minutes). The main differences between microwave and electric firing methods occur in a temperature band of 300°C above the porcelain eutectic temperature (close to 1000°C).     

Non-Uniformity of Surface Temperatures of Grain after Microwave Treatment in an Industrial Microwave Dryer

In this study, temperature rise and non-uniformity of heating of grain with different moisture contents after microwave treatment were investigated. The temperature anomalies after microwave treatment were measured for barley and wheat at four moisture levels (12, 15, 18, and 21% wet basis) and for canola at five moisture levels (8, 12, 15, 18, and 21% wet basis). Fifty grams of grain samples were heated in a laboratory scale, continuous-type, industrial microwave dryer (2450 MHz) at five power levels (100, 200, 300, 400, and 500 W) and two exposure times (28 and 56 s). Grain samples were thermally imaged using an infrared thermal camera as soon as they came out from the microwave chamber. Average, maximum, and minimum temperatures were extracted from each thermal image and the difference between maximum and minimum temperatures (ΔT) was calculated. The grain type had significant effect on the surface temperatures after microwave treatment. The surface temperatures increased with microwave powers and exposure times but decreased with moisture content. The average surface temperatures after microwave treatment were between 72.5 and 117.5°C, 65.9 and 97.5°C, and 73.4 and 108.8°C for barley, canola and wheat, respectively, when the applied microwave power was 500 W. At the same power level, the maximum surface temperature was between 100.3 and 140.0°C, 77.8 and 117.7°C, and 98.3 and 130.9°C for barley, canola, and wheat, respectively. Non-uniform heating patterns were observed for all three grain types at all moisture contents, power levels, and exposure times. The ΔT was in the range of 7.2 to 78.9°C, 3.4 to 59.2°C, and 9.7 to 72.8°C for barley, canola, and wheat, respectively. The location of hot and cold spots may vary in different dryers based on the position of magnetron and other components, but almost similar non-uniform heating pattern is expected in all microwave dryers. Therefore, this non-uniformity must be taken into consideration while developing microwave processing systems for grains.     

Water Absorption Behavior and Impact Properties of Spartium Junceum Fiber Composites

This paper presents the influence of Spartium junceum (SJ) fiber content, surface treatment and temperature on the water uptake of polypropylene/Spartium junceum fiber (PP/SJ) composites. Composites specimens were dried at 70°C to reach a constant weight and then were submerged in distilled water at different temperatures, 23°C and 85°C. Water uptake of PP/SJ fiber composites was found to increase with fiber content. Impact strength properties are dramatically affected by the water absorption. Water-saturated samples present poor impact strength. The SEM micrograph of Spartium junceum fiber untreated and treated with silane (Z-6020) illustrate the reduction of roughness via surface treatment of fiber.     

Development of a new pre-drying method of accelerated water absorption and partial gelatinization of starch in paddy using pulsed microwave-water applications in a microwave rotary drum dryer

The present study was undertaken to develop a pre-drying process of an accelerated water absorption and partial gelatinization of starch in paddy using pulsed microwave-water applications. The experiments on microwave-assisted water absorption by paddy (var. Sworn Masuri) at five power density levels in the range 0.2–1?kW?kg^?1 were conducted in a semi-pilot-scale microwave dryer. The paddy was exposed to pre-calculated intermittent water spray and pulsed microwaves up to 100?min. The water absorption kinetics were modeled using modified Azuara’s equation of mass transfer and the process was compared with traditional hot water soaking of the paddy at 60?°C for 3.33?h. The moisture content gained by paddy during microwave-assisted water absorption was faster (30% in 1.67?h) compared to hot water soaking (30% in 3.33?h). The consumption of water, specific energy, and water absorption time during microwave processing were reduced by 70%, 39.51%, and 50%, respectively. The method of slopes was used to estimate moisture diffusivity during microwave-assisted water absorption by paddy. X-ray diffraction (XRD) analysis and scanning electron microscopy (SEM) of treated paddy were done to understand the changes in the crystallinity and the microstructure of starch molecules. The microwave-assisted water absorption process was found to accelerate the moisture gain with the effect of partial gelatinization of starch in the paddy. Further, the experiment can be continued in the same microwave dryer to fully gelatinize the paddy at 30% moisture content and dry the gelatinized paddy.     

Effect of different thermal treatments on the mechanical performance of poly(L‐lactic acid) based eco‐composites

PLLA‐based eco‐composites reinforced with kenaf fiber and rice straw and containing red or yellow pigments have been studied. The mechanical behavior of the composites was tested by DMTA at two different annealing temperatures (65°C and 85°C) and times (15 min and 120 min) as well as at two preparation conditions: vacuum drying and long time at room temperature. A decrease of microhardness was observed during the water absorption tests. Moreover, the rice straw‐based composites absorbed more water than the kenaf‐ones. Generally, the dyed NFs composites presented better water resistance than undyed ones. The pigments improved the adhesion and led to better mechanical performance. The natural fibers favored the cold crystallization process of PLLA and shifted the cold crystallization peak temperature to lower values, as it was confirmed by DSC measurements. The values of tensile storage modulus obtained after different preparation condition were strongly affected by the process of physical ageing. According to, tan δ parameter, the samples stored at room temperature for a long time showed the highest amorphous content. The PLLA eco‐composite reinforced with kenaf fibers, dyed with the red pigment, and annealed at 85°C for 2 h displays the best mechanical properties. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Studies on the improvement of cured two-stage phenolics performance. III. Relation between conditions of heat treatment and properties of wood-flour-filled phenolics

The effect of heat treatment on the properties of cured two-stage phenolics was studied. Samples were compression-molded from the compound that was prepared from novolac, wood flour (100 phr), and hexamethylenetetramine (15 phr). Samples were heat-treated in conditions of four levels for temperature (150°C, 170°C, 190°C, and 210°C) and time (4, 8, 16, and 24 h). The properties of samples heat-treated, such as weight loss, dimensional stability, water absorption after boiling, and flexural properties were measured. The relation between the properties and the conditions of heat treatment was examined statistically. From the results, it was decided that the optimum conditions of heat treatment for practical use were: (i) to decrease water absorption and to heighten electrical resistance, 210°C, 24 h; (ii) to improve flexural properties at room temperature and at 160°C; 170°C, 8 h, and 170–190°C, 24 h, respectively. It was concluded that the decrease of water absorption of moldings was due to the increase of hydrophobic nature of wood flour included in moldings by heat treatment and that the improvement of flexural property of moldings at 160°C was due to an increase of crosslinking density by heat treatment. The reasons for the improvement of the electrical properties by heat treatment were also discussed.     

Potential of Ozonated Water at Different Temperatures to Improve Safety and Shelf-Life of Fresh Cut Lettuce

The present study was carried out to determine the effect of ozonated water (2 mg L^?1) at different temperatures (4 °C and 15 °C) on the microbiological, color and sensory properties of lettuce. Cold ozone treatment (4 °C) significantly reduced the natural background microflora of lettuce. Salmonella Typhimurium and Escherichia coli inoculated on lettuce samples were insignificantly influenced by the temperature of water. During storage period at +4 °C for 14 days, the highest quality was observed from the samples treated with cold ozonated water. Ozone treatments did not affect the color properties and sensory quality of lettuce samples.     

Global insight into microwave stoneware firing: Macro and microstructural changes

Industrial competition and environmental concerns lead to the exploration of alternative and energy-efficient technologies for ceramic materials processing. The main objective of this work was to present microwave heating as a viable option for stoneware processing. Stoneware functional properties are presented and discussed, with emphasis on impact strength, water absorption, porosity, and color. Microstructure analyses show that microwave- and gas-fired samples have higher densifications than electrically fired samples. A relevant finding for processing conditions is that microwave firing requires temperatures approximately 100°C lower than those required by conventional firing. Microwave-fired samples’ rupture energies are approximately twice (0.57 ± 0.06 (J)) those of the reference samples (0.26 ± 0.03 (J)), and their water absorptions are approximately one-half (1.5% at 1170°C and 0.8% at 1190°C) of those of the reference samples (2.0%), whereas the water absorption of electrically fired samples at 1180°C has been estimated to be 7.5%. Color analysis also evidences a shift to lower microwave firing temperatures, what is attributed to the enhanced transformations promoted by microwave heating when comparing with the transformations promoted by conventional (gas or electric) heating.     

Effect of absorbed water on dynamic modulus for short fiber–CR composites

Short fiber–elastomer composites with 10 vol % fiber, nylon 6–CR and PET–CR composites, absorbed water either in the moisture atmosphere or in water. The effect of absorbed water on the viscoelastic properties for these composites was investigated. The temperature dependence of tan σ for the nylon–CR composite showed that the α-dispersion peak of nylon shifted to lower temperatures with increasing absorbed water content and that after displacement of the α-dispersion peak the additional small hump appeared at about 90°C. For the PET composite, the α-dispersion peak of PET shifted slightly to lower temperatures and the small shoulder at 90°C diminished with increasing absorbed water. The additional dispersion probably was caused by the interface between fiber and CR matrix and was independent of fiber orientation. The results suggested that nylon fiber absorbed a larger amount of water than CR matrix, while the water absorption for PET fiber was considerably less than for nylon fiber. The absorbed water in nylon fiber bonded stronger than that in CR matrix and was only slightly diminished by heat treatment under 100°C.