Showing papers in "Journal of Thermal Analysis and Calorimetry in 1996"

THE GLASS TRANSITION TEMPERATURE OF POLYSTYRENE Results of a round robin test

Abstract: A round robin test was performed to determine the reliability of values for the glass transition temperatureTg as determined by DTA on polymers. Ten different instruments were involved. The test material was high molecular weight polystyrene. Values forTg (midpoint) were reported in the range 107°C±2 K. The respective heat flow curves differed considerably in shape. In the literature aTg of 100°C is often given for polystyrene. The discrepancy between this value and the value of 107°C found in the round robin test is due to three differences: the thermal history of the sample, the evaluation of the heat flow curves, and the effect of finite sample size.

Thermogravimetric and dynamic mechanical thermal analysis of pineapple fibre reinforced polyethylene composites

Abstract: The thermal behaviour of pineapple leaf fibre (PALF) reinforced polyethylene composites was studied by thermogravimetric and dynamic mechanical thermal analysis. Fibre treatment was carried out using isocyanate, silane and peroxide to improve the interfacial adhesion between fibre and matrix. The effects of fibre loading and surface modification on the thermal properties were evaluated. It was found that at high temperature PALF degrades before the polyethylene matrix. The storage modulus increased with increase of fibre loading and decreased with increase of temperature. The treated fibre composites impart better properties compared to untreated system. Tan δ showed a distinct peak at low temperature ascribed to the glass transition temperature of polyethylene but no peak was observed for PALF fibre. The relative damping increased with fibre loading. Cole-Cole analysis was made to understand the phase behaviour of the composite samples.

The effects of co-lyophilized polymeric additives on the glass transition temperature and crystallization of amorphous sucrose

Abstract: The purpose of this study was to measure the effect of co-lyophilized polymers on the crystallization of amorphous sucrose, and to test for a possible relationship between the ability of an additive to raise theT g of a sucrose-additive mixture, relative to theT g of pure sucrose, and its ability to inhibit crystallization. Differential scanning calorimetry was used to measure the glass transition temperature,T g, the non-isothermal crystallization temperature,T c, and the induction time for crystallization,Q, of sucrose in the presence of co-lyophilized Ficoll or poly(vinylpyrrolidone) (PVP). The effect of these polymers on the crystallization of sucrose was significant as demonstrated by a marked increase inT c, and in the induction time (Q) in the presence of relatively small amounts (1–10%) of additive. Surprisingly, small amounts of polymeric additive had no effect on theT g of sucrose, although at higher concentrations, theT g increased proportionally. Thus, it appears that the inhibition of sucrose crystallization by the additition of small amounts of a higher-T g component cannot be attributed solely to changes in molecular mobility associated with an increase inT g.

Temperature modulated calorimetry and dielectric spectroscopy in the glass transition region of polymers

Abstract: The results from temperature modulated DSC in the glass transition region of amorphous and semicrystalline polymers are described with the linear response approach. The real and the imaginary part of the complex heat capacity are discussed. The findings are compared with those of dielectric spectroscopy. The frequency dependent glass transition temperature can be fitted with a VFT-equation. The transition frequencies are decreased by 0.5 to 1 orders of magnitude compared to dielectric measurements. Cooling rates from standard DSC are transformed into frequencies. The glass transition temperatures are also approximated by the VFT-fit from the temperature modulated measurements. The differences in the shape of the curves from amorphous and semicrystalline samples are discussed.

Dielectric spectroscopy and calorimetry in the glass transition region of semi-crystalline poly(ethylene terephthalate)

Abstract: Confinement of the glass-forming regions in the nanometer range influences the α-relaxation which is associated with the glass transition. These effects were investigated for semicrystalline poly(ethylene terephthalate) by dielectric spectroscopy and differential scanning calorimetry. The results are discussed within the concept of cooperative length, i.e. the characteristic length of the cooperative process of glass transition. Both experiments showed a dependence of the glass transition on the mean thickness of the amorphous layers. For the dielectric relaxation, the loss maximum was found to shift to higher temperatures with decreasing thickness of the amorphous layers, but no differences were observed in the curve shape for the differently crystallized samples. For the calorimetric measurements, in contrast, there was no correlation for the glass transition temperature, whereas the curve shape did correlate with the layer thickness of the mobile amorphous fraction. From the structure parameters, a characteristic length of approximately (2.5±1) nm was estimated for the unconfined glass relaxation (transition).

Influence of heating and cooling rates on the glass transition temperature and the fragility parameter of sorbitol and fructose as measured by DSC

Abstract: The glass transition temperatures of sorbitol and fructose were characterized by four points determined on DSC heating thermograms (onset, mid-point, peak and end-point), plus the limit fictive temperature. The variations of these temperature values, observed as functions of cooling and heating rates, were used to determine the fragility parameter, as defined by Angell [1] to characterize the temperature dependence of the dynamic behavior of glass-forming liquids in the temperature range above the glass transition.

Liquid crystalline polymers

Abstract: The suitabilities of thermo-optometry and differential scanning calorimetry for the characterization of certain copolyethers were compared Under certain conditions, such polymers do not exhibit the endotherm signal corresponding to the solid/liquid crystalline transition in the DSC curves Thermo-optometry provides evidence of these phase transitions into the liquid crystalline state, and is a very useful additional method

Vitrification of trehalose by water loss from its crystalline dihydrate

Abstract: Trehalose dihydrate, on careful dehydration below its fusion point, retains its original crystal facets but becomes X-ray amorphous, an unusual example of direct crystal-to-glass transformation. From DSC studies, the glass obtained by this route seems to be of abnormally low enthalpy, but after an initial scan, the normal form of glass transition is exhibited, withTg=115‡C, a higher value than previously reported. We give a preliminary thermal and mechanical characterization of this material and find it to be a very fragile liquid. The highTg is shown to rationalize the exceptionally high water content of the trehalose+water solution that vitrifies at ambient temperature (i.e.Tg=298 K), and hence helps explain its use by Nature as a desiccation protectant. The spontaneous vitrification of crystalline materials during desolvation is related to the phenomenology of pressure-induced or decompression-induced vitrification of crystals via the concept of limiting metastability.

Effect of hydrocolloids on starch thermal transitions, as measured by DSC

Abstract: Differential scanning calorimetry (DSC) was used to analyze the influence of different hydrocolloids (xanthan, guar, and locust bean gums, carboxymethylcellulose and sodium alginate) on the gelatinization of corn starch in systems with starch concentration ranging between 0.1 and 0.7 g starch/g mixture. The reduction of available water produced a shift in gelatinization temperature, especially of the conclusion temperature. The effect was more marked for ionic hydrocolloids. The influence of hydrocolloids on glass transition temperature (Tg) of gelatinized starch suspensions and on the glass transition temperature of the maximally freeze-concentrated solute/unfrozen water matrix (T′g) was also studied.T′g onset values ranged between −4.5 and −5.5‡C for corn starch pastes with and without hydrocolloids. Those hydrocolloids that increased the viscosity of the unfrozen matrix inhibited additional ice formation during thawing (devitrification).

Thermal degradation of ethylene (vinyl acetate)

Abstract: Ethylene (vinyl acetate), EVA, is a copolymer which is thermally degraded at high temperatures, with acetic acid release at approximately 620 K. This release can be studied by using thermal methods, and in particular thermogravimetric analysis.

Dynamic DSC, SAXS and WAXS on homogeneous ethylene-propylene and ethylene-octene copolymers with high comonomer contents

Abstract: Ethylene-propylene (EP) and ethylene-octene (EO) copolymers polymerized with the aid of homogeneous vanadium and metallocene catalysts were compared by DSC and time-resolved simultaneous SAXS-WAXS-DSC at scanning rates of 10 and 20°C min−1 using synchrotron radiation. An EP copolymer with a density of 896 kg m−3 (about 89 mol % ethylene) after compression moulding gave orthorhombic WAXS reflections. The crystallinity as a function of temperature [wc(T)] calculated from these reflections using the two-phase model was in good agreement withwc(T) calculated fromcp measurements using DSC. Thecp measurements also enabled calculation of the baselinecp and the excesscp. The SAXS measurements revealed a strong change in the long period in cooling and in heating. The SAXS invariant as a function of temperature showed a maximum in both cooling and heating, which could be explained from the opposing influences of the crystallinity and the electron density difference between the two phases. Two EO copolymers with densities of about 871 kg m−3 (about 87 mol% ethylene) no longer showed any clear WAXS reflections, although DSC and SAXS measurements showed that these copolymers did crystallize. The similarity between the results led to the conclusion that the copolymers, though based on different catalyst systems — vanadium and metallocene — did not have strongly different sets of propagation probabilities of chain growth during polymerization. On the basis of a Monte Carlo simulation model of crystallization and morphology, based on detailed knowledge of the microchain structure, the difference between WAXS on the one hand and DSC and SAXS on the other could be explained as being due to loosely packed crystallized ethylene sequences in clusters. These do cause the density and the electron density of the cluster to increase (which is measurable by SAXS) and the enthalpy to decrease (which is measurable by DSC) but the clusters are too small and/or too imperfect to give constructive interference in the case of WAXS. Of an EP copolymer with an even lower ethylene content (about 69 mol %), the crystallization and melting processes could still be readily measured by DSC and SAXS, which proves that these techniques are eminently suitable for investigating the crystallization and melting behaviour of the copolymers studied.

Thermal transitions of cassava starch at intermediate water contents

Abstract: Order-disorder transitions were investigated in native cassava starch at intermediate moisture contents (35 to 60% wt. water), using Differential Scanning Calorimetry (DSC) and dynamic Wide Angle X-ray Diffractometry (WAXS) with a synchrotron radiation source.

Isothermal microcalorimetric studies on starch retrogradation

Abstract: In the present study, isothermal microcalorimetry was introduced as a tool to investigate properties of starch retrogradation during the first 24 h. The study was made on purified amylose and amylopectin from corn, as well as on native starches, such as wheat, potato, maize, waxy maize and amylomaize, differing in their amylose content. The results were obtained in the form ofP-t traces (thermal powervs. time), and integration of these traces gave a net exothermic enthalpy of reaction, caused by the crystallization of amylose and amylopectin. TheP-t traces reflected the quantities of amylose and amylopectin in the starch studied. Depending on the amylose content and the botanical source of the starch, the rate of crystallization of amylose was high and predominated over that of amylopectin during the first 5–10 h. The contribution from amylose crystallization to the measured exothermic enthalpy was very substantial during this period. After ∼10 h, amylose crystallized at a lower constant rate. During the first 24 h, amylopectin crystallized at a low steady rate. The exothermic enthalpies obtained by the isothermal microcalorimetric investigations during the first 24 h of retrogradation were generally low in relation to the endothermic melting enthalpies observed by differential scanning calorimetry (DSC) measurements after 24 h of storage. The discrepancies in enthalpy values between the two methods are discussed in relation to phase separation and the endothermic effects owing to the decrease in polymer-water interactions when polymer-rich regions in the starch gel separate. Besides the exothermic enthalpies obtained, theP-t traces also made it possible to study the initial gelation properties of amylose from different botanical sources. The present study further demonstrated that isothermal microcalorimetry can provide a possible way to investigate the antistaling effect of certain polar lipids, such as sodium dodecylsulphate (SDS) and 1-monolauroyl-rac-glycerol (GML), when added to starches of different botanical origin. The net exothermic heat of reaction for starch retrogradation during the first 24 h was decreased when GML or SDS was added to the starch gels. The recordedP-t traces also showed how the effect of the added lipid influenced different periods during the first 24 h of starch retrogradation, and that the effect depended mainly on the amylose content, the botanical source of the starch, and the type of lipid used. When GML or SDS was added to waxy maize, the isothermal microcalorimetric studies clearly indicated some interaction between amylopectin and the polar lipids. These results concerning the action of anti-staling agents are further discussed in relation to the helical inclusion complexes formed between amylose-polar lipid and amylopectin-polar lipid.

Thermomechanical properties of glassy cereal foods

Abstract: The main objective of this paper is to discuss the relationship between physical state, fracture mechanism, and texture for low moisture cereal-based foods. Experiments were also carried out to get a better understanding of the role of water. At room temperature, extruded bread and white bread (previously) dehydrated, then rehydrated in atmospheres with controlled humidities) exhibited a brittle behavior up to around 9% moisture. At 13.7% moisture, they were ductile. A significant loss in the crispness of extruded bread was observed between 8.5 and 10% moisture. The glass transition temperature (Tg) was measured, using dynamic mechanical thermal analysis (DMTA), for samples with up to 40% moisture. The resultingTg curve showed that the important changes in fracture mechanisms and crispness occurred while the samples were still in the glassy state. The viscoelastic behavior of both extruded and white breads suggested that a secondary relaxation occurred around 10‡C. Another event was observed around 70‡C for low moisture sample, using DMTA. This event was attributed to disruption of low energy interactions.

Crystallization, melting and spherulitic structure of Β-nucleated random propylene copolymers

Abstract: The characteristics of crystallization, melting and spherulitic growth of a random propylene copolymer (PRC) containing small amount of ethylene were studied in the presence of a selective Β-nucleating agent (calcium pimelate). It was established that the products of isothermal and non-isothermal crystallization are very rich in Β-modification but have mixed polymorphic composition. The formation of α-modification may be attributed to Βα-transition on the surface of growing Β-spherulites resulting in αΒ-twin-spherulites. During melting of PRC of Β-modification, the characteristics observed with Β-nucleated propylene homopolymers, namely, a Βα-recrystallization of recooled samples and separated melting of non-recooled samples (i.e. the melting memory effect), as well as a ΒΒ-recrystallization leading to a perfection of the structure within the Β-modification, are also demonstrated. The disturbance of regularity of the polymer chain highly reduces the tendency to Β-crystallization. In contrast to the observ...

Some problems concerning the evaluation of non-isothermal kinetic parameters

Abstract: The validity of isoconversional methods used to evaluate the activation energy is discussed. The authors have shown that the Flynn-Wall-Ozawa and Friedman methods give results that agree with each other only if the activation energy does not change with the degree of conversion. A criterion for the reaction mechanism as expressed by the differential conversion function is suggested too.

Differential thermal analysis of montmorillonite

Abstract: The paper provides an overview of publications on the DTA of montmorillonites (in the temperature range 20–1100°C), starting with the first experiments of Le Chatelier (1887) and ranging up to the present. Consideration is given to the dehydration, dehydroxylation, amorphization and rehydration of montmorillonite (42 references).

Investigation of the complex thermal behavior of fats

Abstract: The thermal behavior of three ural fats (displaying very different composition), cocoa butter (CB)2, lard, and a stearin obtained from anhydrous milk-fat (AMF) fractionation, were studied by both DSC and X-ray diffraction as a function of temperature (XRDT). To perform temperature explorations between −30‡C and +80‡C, at rates identical to those used for DSC and ranging from 0.1 K min−1 to 10 K min−1, a new set of X-ray sample-holders, temperature-controlled by Peltier effect, has been developed. It is shown that the three more stable polymorphic forms of CB were easily characterized by either X-ray diffraction or DSC, and existence of two Β-3L forms was confirmed. On the contrary, the more complex polymorphism of lard and AMF required combined examination by DSC and XRDT and the brightness of the synchrotron source for studies at the highest heating rates. Quantitative analysis of the long spacings of XRDT recordings is invaluable for interpretation of thermal events. For instance, it was found that the simultaneous formation of two polymorphic forms, of apparent long spacing of 34 and 42 a, at the onset of lard crystallization might explain the difficulty of its fractionation.

NON-ENZYMATIC BROWNING-INDUCED WATER PLASTICIZATION Glass transition temperature depression and reaction kinetics determination using DSC

Abstract: An exotherm, observed in differential scanning calorimetry (DSC) scans of amorphous food materials above their glass transition temperature,T g, may occur due to sugar crystallization, nonenzymatic browning, or both. In the present study, this exothermal phenomenon in initially anhydrous skim milk and lactose-hydrolyzed skim milk was considered to occur due to browning during isothermal holding at various temperatures above the initialT g. The nonenzymatic, Maillard browning reaction produces water that in amorphous foods, may plasticize the material and reduceT g. The assumption was that quantification of formation of water from theT g depression, which should not be observed as a result of crystallization under anhydrous conditions, can be used to determine kinetics of the nonenzymatic browning reaction. The formation of water was found to be substantial, and the amount formed could be quantified from theT g measured after isothermal treatment at various temperatures using DSC. The rate of water formation followed zero-order kinetics, and its temperature dependence well aboveT g was Arrhenius-type. Although water plasticization of the material occurred during the reaction, and there was a dynamic change in the temperature differenceT−T g, the browning reaction was probably diffusioncontrolled in anhydrous skim milk in the vicinity of theT g of lactose. This could be observed from a significant increase in activation energy. The kinetics and temperature dependence of the Maillard reaction in skim milk and lactose-hydrolyzed skim milk were of similar type well above the initialT g. The difference in temperature dependence in theT g region of lactose, but above that of lactose-hydrolyzed skim milk, became significant, as the rate in skim milk, but not in lactose-hydrolyzed skim milk, became diffusion-controlled. The results showed that rates of diffusion-controlled reactions may follow the Williams-Landel-Ferry (WLF) equation, as kinetic restrictions become apparent within amorphous materials in reactions exhibiting high rates at the same temperature under non-diffusion-controlled conditions.

Thermal dehydration and decomposition of FeCl3·xH2O

Abstract: Thermal dehydration and decomposition characteristics of Fe(III) chloride hydrate have been studied by both isothermal and non-isothermal methods. After the initial melting at 35–40°C both dehydration and decomposition of the salt proceed simultaneously at temperature above 100°C. At 250–300°C a stable hydrated Fe(OH)2Cl is formed representing the first plateau region in the TG curve. Around 400°C, a second plateau is observed corresponding to the formation of mostly Fe2O3 which however retains some OH groups and Cl− ions. However, these temperature ranges vary with the TA equipments used. Chemical analysis of the products of decomposition at temperatures above 140°C also gives evidence for the formation of FeOCl which on hydrolysis in water gives FeCl3 in solution. The FT-IR spectra suggest the presence of structural OH groups even for samples calcined at 300–400°C. The XRD patterns of the products of decomposition in the temperature range 160–400°C indicate the presence of β-FeOOH, some unidentified basic chlorides and α-Fe2O3.

Thermal decomposition of Ni(II) and Fe(III) acetates and their mixture

Abstract: The thermal decomposition of the ferric and nickel acetate salts has been followed. It was found that the heating rate affects the decomposition steps. For a heating rate of 1 K min−1 the product is either Fe2O3 or NiO. For a higher heating rate the suboxides are obtained and reoxidized again on further heating. The decomposition of the mixed salt is an overlap of the DTA for the separate salts but the decomposition reactions are shifted to lower temperatures.

Structural collapse of plant materials during freeze-drying

Abstract: Structural collapse of plant materials, which affects quality of foods, was studied. Fresh and osmotically dehydrated plant materials were freeze-dried at several chamber pressures, to achieve initial sample temperatures that were below (−55‡C), near (−45‡C), or above (−28‡C) their glass transition temperature (Tg=−45‡C). Freeze-drying at −55‡C resulted in products retaining their original volume. When the initial sample temperature was increased aboveTg, the resulting freeze-dried samples collapsed. When the initial sample temperature was increased above the temperature of ice melting (T′m), the samples collapsed further.

Thermogravimetric analysis for boiling points and vapour pressure

Abstract: A TGA instrument has been adapted for rapid measurement of boiling points and vapour pressure at temperatures from ambient up to 400°C and pressures from ambient down to 20 mm Hg. Samples were contained in sealed holders having a laser-drilled aperture. Several organic liquids in the 100 to 300 gMW range showed good agreement with reference vapour pressure data. Sample mass, heating rate, and use of inert diluents were important variables affecting accuracy of vapour pressure measurements.

Application of differential scanning calorimetry in food research and food quality assurance

Abstract: Differential scanning calorimetry (DSC) is the most widely used thermal analytical technique in food research and it has a great utility in quality assurance of food. Proteins are the most studied food components by thermal analysis including studies on conformation changes of food proteins as affected by various environmental factors, thermal denaturation of tissue proteins, food enzymes and enzyme preparations for the food industry, as well as effects of various additives on their thermal properties. Freezing-induced denaturation of food proteins and the effect of cryoprotectants are also monitored by DSC. Polymer characterization based on DSC of polysaccharides, gelatinization behaviour of starches and interaction of starch with other food components can be determined, and phase transitions during baking processes can be studied by DSC. Studies on crystallization and melting behaviour of fats observed by DSC indicate changes in lipid composition or help characterizing products. Thermal oxidative decomposition of edible oils examined by DSC can be used for predicting oil stability. Using DSC in the freezing range has a great potential for measuring and modelling frozen food thermal properties, and to estimate the state of water in foods and food ingredients. Research in food microbiology utilizes DSC in better understanding thermoadaptive mechanisms or heat killing of food-borne microorganisms. Isothermic microcalorimetric techniques provide informative data regarding microbial growth and microbial metabolism.

A computer-controlled apparatus for thermal conductivity measurement by the transient hot wire method

Abstract: The aim of this paper is to review the transient hot wire method for measurement of thermal conductivity, which is based on the measurement of temporal history of the temperature rise caused by linear heat source (hot wire) embedded in a test material. If a current is passed through the wire, the rise in temperature will be dependent, among other factors, on the thermal conductivity of the medium, surrounding the wire. Here the mathematical basis, as well as main modifications of the hot wire method — cross technique, resistance modifications with potential and compensated lead methods; hot wire probe method and parallel wire technique, are described and discussed. A fully automated computer-controlled transient hot wire apparatus is presented and tested, which allows measurement of thermal conductivity of solid, powder and granular materials at high temperatures.

Modulated differential scanning calorimetry in the glass transition region: II. The mathematical treatment of the kinetics of the glass transition

Abstract: Temperature-modulated differential scanning calorimetry (TMDSC) is based on heat flow and represents a linear system for the measurement of heat capacity. As long as the measurements are carried out close to steady state and only a negligible temperature gradient exists within the sample, quantitative data can be gathered as a function of modulation frequency. Applied to the glass transition, such measurements permit the determination the kinetic parameters of the material. Based on either the hole theory of liquids or irreversible thermodynamics, the necessary equations are derived to describe the apparent heat capacity as a function of frequency.

Transformations of manganese oxides under different thermal conditions

Abstract: Thermal decomposition of various synthetic manganese oxides (MnO, Mn3O4, Mn2O3, MnOOH) and a natural manganese dioxide (MnO2) from Gabon was studied with the help of termogravimetry in inert, oxidizing and reducing atmospheres. The compounds were characterized by XRD and electrochemical activity was tested by cyclic voltammetry using a carbon paste electrode. The natural manganese dioxide showed the best oxidizing and reducing capacity, confirmed by the lower temperatures of the transitions, the extent of the reactions and electrochemical performance in cyclic voltammograms.

Modulated temperature DSC measurements relating to the cold crystallization process of poly(ethylene terephtalate)

Abstract: The modulated temperature differential scanning calorimetric method (MT-DSC) yields three temperature dependent signals, an underlying heat capacity curve from the underlying heat flow rate (corresponding to the conventional DSC signal), and a complex heat capacity curve with a real part (storage heat capacity) and an imaginary part (loss heat capacity). These curves have been measured in the cold crystallization region for poly(ethylene terephtalate) with a modified Perkin-Elmer DSC-7. The underlying curve shows the well known large exothermic crystallization peak. The storage heat capacity shows a step change which reproduces the change in heat capacity during crystallization. This curve may be used as baseline, to separate the crystallization heat flow rate from the underlying heat flow rate curve. The loss heat capacity curve exhibits a small exothermic peak at the temperature of the step change of the storage curve. It could be caused by changes of the molecular mobility during crystallization.

Effect of hydrothermal treatment on the gelatinisation properties of potato starch as measured by differential scanning calorimetry

Abstract: Gelatinisation temperatures as a function of moisture content were determined for potato starch. The native starch was then hydrothermally treated at a temperature 3% (Kelvin degrees) below the gelatinisation peak temperature and at moisture levels varying from 20 to 67% (by weight). Gelatinisation temperatures, temperature ranges and enthalpy values were affected for all treated samples. However, two sample populations could be distinguished: those samples treated under ‘limited’ moisture conditions and other samples treated in the presence of ‘extragranular’ moisture. A two-step hydrothermal treatment further increased the gelatinisation temperature, but the effect of the second step was small in comparison to that of the first.

Construction of a wheat-flour state diagram

Abstract: We use pressure-variable differential scanning calorimetry to detect and characterize thermally induced transitions (glass, melting, gelatinization) in pre- and post-extruded wheat flour. The resulting data allow us to construct a two-dimensional state diagram which maps the physical states that pre- and post-extruded wheat flour can assume, at constant pressure, as a function of moisture content, temperature, and the specific mechanical energy, SME, generated in the extruder. We describe how this state diagram can be used to map the path of extrusion processing, to assess the impact of extrusion conditions, and, ultimately, to design formulations and processing conditions that result in desired end-product attributes. For the extrudates, we find that the extent of processing-induced fragmentation, as monitored by reductions in the extrudate glass transition temperature,Tg, increases with the SME generated in the extruder. We demonstrate that a wheat-flour state diagram, which includes the glass curve of the wheat-flour extrudates produced at various SME values, allows one to predict and control the impact of processing conditions on extrudate properties.