Measurement of rheological and ultrasonic properties of food and synthetic polymer melts

A slit die viscometer has been used in conjunction with a co-rotating twin screw extruder to study the rheological behaviour of maize grits, potato powder and low density polyethylene, as a function of feed rate, screw speed and temperature. The shear viscosity of both maize and potato decreased with increasing feed rate. Increasing the temperature or screw speed at any given feed rate also reduced the viscosity. The ultrasonic velocity through the material has also been shown to be sensitive to the extruder operating conditions. Overall, the ultrasonic velocity decreased as screw speed and temperature increased and feed rate decreased.     

Viscosity of some clay-based coating colors at high shear rates

The shear viscosity of clay-based coating colors containing latex and carboxymethyl cellulose (CMC) has been measured over a relatively large shearrate region. In the shear-rate range of 50–1500 s^–1 the measurements were performed using a rotational viscometer and, at higher shear rates extending into the region 10⁵ – 10⁶ s^–1, a high pressure capillary viscometer was employed. The viscosity of the clay colors increased with increasing CMC-concentration, but the influence of the CMC-content was less pronounced at higher shear rates. The apparent shear-thinning behavior of the investigated colors could, in part, be attributed to the shear-thinning of the corresponding polymer (CMC) solution constituting the liquid phase of the color, but the influence of another factor was also indicated. At low shear rates, the interaction between the color components can produce relatively high viscosity levels, but in the high shear rate region these interactions appear to be less important for the viscosity level. It is also of interest to note that the viscosity dependence on the solids content in the high shear-rate region could be described with reasonable accuracy using an empirical equation neglecting interactions between the color components.     

Drilling fluid shear stress overshoot behavior

Shear stress overshoot behavior was studied in four drilling fluid systems and ten bentonite dispersions. These overshoot properties, also described by the American Petroleum Institute as gel strengths, were measured after gelation times of 10 s to 24 h at temperatures of 20–80 °C. Two different rheometers were used to measure overshoot behavior. Gel strength development with time followed a first-order model. Gel development rates at 20 °C varied from 0.005 to 0.01 min^–1 for drilling fluid systems and from 0.0004 to 0.02 min^–1 for bentonite dispersions. Increasing the gelation temperature for each drilling fluid system caused an increase in the gelling rate constant. Comparison of gel strengths in bentonite dispersions were made using a Fann 35 A viscometer and a Weissenberg Rheogoniometer. Higher gel strength values observed using the Rheogoniometer were believed to be due to differences in instrument spring stiffness and fixture inertia.     

A slit viscometer for the measurement of the viscosity of aqueous systems at high temperatures

A slit viscometer has been constructed to measure the viscosity of aqueous systems at temperatures up to 140 °C. Liquid is forced backwards and forwards through the slit by the use of varying air pressure. The flow rate is obtained from the time for the liquid to pass conductivity probes located in liquid reservoirs either side of the slit. The pressure difference between two points on the slit wall is determined using a differential pressure transducer. By varying the slit height measurements can be made on liquids with viscosities in the range 10 to 10^–3 Pa s. Shear rates from 10 to 10⁴ s^–1 can be achieved. A simple microcomputer control system enables the shear stress to be automatically increased and decreased stepwise. Representative data on polysaccharide solutions and strach suspensions are presented. The viscometer is particularly well-suited for following temperature-dependent biopolymer transitions and the thermal depolymerisation of water soluble polymers.     

Shear and extensional flow of polyacrylamide solutions

As part of an EEC Science Stimulation programme on extensional viscosity two major conferences were organised on the subject. The second of these was devoted to the results obtained on a standard fluid, M 1. The data obtained in shear flow was remarkably consistent from laboratory to laboratory. Extensional flow results presented quite a different picture. Using a series of nonequilibrium techniques such as the spinline rheometer, opposing jet, falling drop and converging flow, extensional viscosity results were obtained which differed by as much as two to three orders of magnitude. Nevertheless, it was apparent that consistancy did exist between similar techniques. It is in the context of this information that the measurements described below have been made.The shear and extensional flow properties of partially ionised polyacrylamide in solution at concentrations ranging from 5 ppm were measured. The method of solution preparation was found to have a profound effect on the behaviour of the solutions in shear flow. The influence of salt concentration and pH was investigated and is discussed in the context of molecular shape in solution.Extensional flow measurements, using the spinline rheometer, show that the solutions are strongly strain thickening even at concentrations as low as 5 ppm. These results are considered in the light of polymer entanglement and association in the strong flow field.Delivered as a Keynote Lecture at the Golden Jubilee Conference of the British Society of Rheology and Third European Rheology Conference, Edinburgh, 3–7 September, 1990.     

An automated dynamic viscometer with air bearing and inductive transducers for angular displacement detection

A dynamic viscometer is described, with which the dynamic moduli in the frequency range from 2 × 10^–3 to 10 Hz can be determined for liquids with 10^–3 Pa< |G ^* | <10² Pa. Due to the application of an air bearing and inductive transducers for the detection of the angular displacement of both the drive and the measuring cylinder a sensitive apparatus has been made. Very small strains (₀ 10^–3) can be applied and only a small amount of sample (4 ml) is needed. The operation of the apparatus is fully computer-controlled, thus, long runs at various frequencies and temperatures are possible without operator intervention. The theoretical background, calibration procedure, and operation window are described. A presentation of some measurements on two polyisoprene/polystyrene triblock copolymer solutions concludes the work.     

Using regularization methods for the determination of relaxation and retardation spectra of polymeric liquids

The application of Tikhonov regularization to the determination of relaxation and retardation spectra of viscoelastic fluids is discussed using simulated and real experimental data. It is thereby shown that with this method consistent results for relaxation and retardation spectra can be obtained from experimental data for different material functions. Furthermore, the differences between the most frequently used variants of Tikhonov regularization and the maximum entropy method are discussed. For most calculations the program FTIKREG has been used, which is an especially fast and reliable implementation of Tikhonov's regularization method.     

Rheological characteristics of sewage sludge: A granuloviscous material

Problems have been experienced in the screw conveying of a centrifuge dewatered sewage sludge, at about 66% by weight water content. The rheology of the sludge was therefore tested in a viscometer in which the normal stress between the platens could be controlled. Rough platens were used to measure internal shear strengths while smooth steel platens were used to study wall slip.The sludge displayed a number of the characteristics of a granuloviscous material. It was found to possess high initial shear strength, but rapidly softened with shear to lower steady-state strengths. The initial shear strength increased with increasing normal stress, indicating that the sludge was frictional. The initial strength was lower against the smooth platen.The steady-state shear strengths were both rate and stress dependent using the rough platen, and this internal shear strength could be described by a frictional pseudoplastic equation. Using the smooth platen the material was nearly rate independent, and was best described by a Coulomb friction equation. At the higher rates the wall shear strengths were lower than the internal shear strengths.The strengths (both initial and steady-state) were characterised by a high degree of variability from sample to sample, and also showed marked hysteresis with the rough platen. They did not show any consistent variation with moisture content.In terms of screw conveying, the major conclusion is that smooth walls to the flights of the screw and barrel of the conveyor are desirable.     

An experimental study of food melt rheology

The shear viscosity of commercial maize grits, potato powder and a low density polyethylene has been measured under a range of extrusion processing conditions using an extruder-fed slit die viscometer and a capillary rheometer. The results show the strong dependence of the viscosity of food melts on the processing history undergone during extrusion. To this end, the shear viscosity data for the food materials have been fitted to relationships including the effects of temperature, shear rate and moisture. The effect of the shear processing history on the viscosity has been represented by a power-law relationship with extruder screw speed.     

Bimodal model of slurry viscosity with application to coal-slurries. Part 1. Theory and experiment

The rheological behavior of stable slurries is shown to be characterized by a bimodal model that represents a slurry as made up of a coarse fraction and a colloidal size fine fraction. According to the model, the two fractions behave independently of each other, and the non-Newtonian behavior of the viscosity is solely caused by the colloidal fraction, while the coarse fraction increases the viscosity level through hydrodynamic interactions. Data from experiments run with colloidal coal particles of about 2–3 µm average size dispersed in water show the viscosity of these colloidal suspensions to exhibit a highly shearrate-dependent behavior and, in the high shear limit, to match very closely the viscosity of suspensions of uniform size rigid spheres although the coal volume fraction must be determined semi-empirically. Different amounts of coarse coal particles are added to the colloidal suspension and the viscosity of the truly bimodal slurries measured as a function of shear rate. In agreement with the bimodal model, the measured shear viscosities show the coarse fraction to behave independently of the colloidal fraction and its contribution to the viscosity rise to be independent of the shear rate. It is shown that the shear rate exerted on the colloidal fraction is higher than that applied by the viscometer as a result of hydrodynamic interactions between the coarse particles, and that it is this effective higher shear rate which is necessary to apply in the correlations. For determining the coal volume fraction a relatively simple and quite accurate measurement technique is developed for determining the density and void fraction of coarse porous particles; the technique directly relates volume fraction to mass fraction.     

Bimodal model of slurry viscosity with application to coal-slurries. Part 2. High shear limit behavior

It is shown that in a truly bimodal coal-water slurry the hydrodynamic interactions between the coarse particles impose on the fine fraction a shear rate higher than that applied externally by the viscometer walls. A semi-empirical function of the coarse volume fraction is obtained for this correction factor to the applied shear rate. The derivation of this shear correction factor is based on lubrication concepts and introduces the maximum packing fraction,ø _m, at which flow can take place.ø _m is obtainable from a simple dry packing experiment. It is shown that the contribution of the coarse particles to the viscosity rise can be successfully described by a viscosity model employing the same concepts used to derive the shear correction factor. The bimodal model is applied in the high shear limit to polymodal coal slurries with a continuous particle size distribution. In the model, the contribution of the coarse particles to the viscosity rise is taken from separate viscosity measurements for the coarse coal particles, while the contribution to the viscosity of the fine coal particles is taken to be that given by the measured viscosity of colloidal suspensions of monomodal rigid spheres. It is shown that there is a ratio of coarse to fine fraction volumes in the continuous size distribution, corresponding to a specific separating particle size, for which the measured viscosities of the polymodal slurries match almost perfectly over the whole solids volume fraction range with the viscosity values obtained using the bimodal approach. The match is found to be relatively insensitive to the precise value of the separating particle size.     

The role of short chain molecules for the rheology of polystyrene melts.

Atactic polystyrenes of narrow molar mass distribution with average molar masses larger than the critical molar massM _c were mixed with similar polystyrenes of molecular masses lower thanM _c . Linear viscoelastic melt properties of these binary blends were measured with a dynamic viscometer of the concentric cylinder type. One of the experimental findings is that the time-temperature shift factorsa _T are dependent on the composition of the samples. This can be understood, if free volume due to chain-ends is taken into account. A computer-fitted WLF-equation being modified in a proper way leads to the following results: At the glass-transition-temperature the fraction of free volume in polystyrene of infinite molar mass is only 0.015. At a temperature of 180 °C the mean value of the free volume at a chain end is 0.029 nm³ for the polystyrene investigated.     

Measurement of the shear viscosity using a newly developed GRLDA-viscometer

A two-point laser-Doppler anemometer is used to determine velocity gradients. Measuring additionally the pressure drop in channel flow allows one to use this instrument as a viscometer. This is demonstrated by measuring two polymer solutions as well as water. Besides the velocity gradient, the system also furnishes the velocity as well as velocity fluctuations. For surfactant solutions the sudden increase in these fluctuations go hand-in-hand with the sudden shear thickening reported. This behavior thus seems to be caused by a change in type of flow field (structural turbulence) rather than a change in the rheology of the surfactant solutions.This paper is dedicated to Professor Hanswalter Giesekus on the occasion of his retirement as Editor of Rheologica Acta.     

Relaxation dynamics of selected polymer chain segments and comparison with theoretical models

Simultaneous measurement of infrared dichroism and birefringence is used to study selected polymer segment dynamics in isotopically labeled block copolymers. Two different polymers were studied: polybutadiene and poly (ethylene propylene). The first type consisted of a triblock with a short middle block labeled and a diblock with a short end block labeled, while the second type consisted of a triblock with three equal blocks and the end blocks labeled. Results of step strain experiments at –10°C for polybutadiene and at room temperature for poly(ethylene propylene) indicated that segments located at chain ends relax faster than segments located at chain centers. These experimental data were compared to the predictions of two molecular models: the bead-spring model of Rouse and the tube model of Doi and Edwards, and it was found that both models correctly predict the qualitative features of segmental relaxation. However, the tube-model predictions were closer to the experimental results. In addition, when the effects of orientational coupling interactions between segments in the melt were incorporated into this model, its predictions quantitatively agreed with the experimental results. The orientational coupling coefficient for poly(ethylene propylene) was 0.45 as measured from previous work, and for polybutadiene it was found to be 0.4.Delivered as a Keynote Lecture at the Golden Jubilee Conference of the British Society of Rheology and Third European Rheology Conference, Edinburgh, 3–7 September, 1990.Dedicated to Prof. R.S. Stein, University of Massachussets at Amherst, USA, on the occasion of his 65th birthday.     

Etude du régime de mise en mouvement dans un viscosimètre de Couette à cylindres coaxiaux

Résumé L'utilisation du viscosimètre de Couette à cylindres coaxiaux pour l'évaluation des propriétés rhéologiques et l'établissement de la loi d'écoulement des fluides nécessite généralement la connaissance du taux des cisaillement en chaque point de l'entrefer et à tout instant. Cette quantité en général inconnue peut être approchée par des expressions mathématiques satisfaisantes pour l'écoulement à couple appliqué mais d'autant plus grossières qu'on s'éloigne du régime stationnaire pour l'écoulement à vitesse imposée. La plupart des approximations généralement utilisées sont obtenues sous l'hypothèse d'un fluide dont n'influence pas l'écoulement et pour un entrefer petit. Notre travail étudie la limite de validité de certaines approximations du taux de cisaillement pour l'écoulement transitoire à vitesse imposée. Dans le contexte de la mise an évidence des propriétés viscoélastiques de certains fluides nous avons choisi d'étudier l'écoulement de montée en vitesse plus utilisé que l'écoulement de relaxation sur l'exemple d'un fluide de type Maxwell. Nous montrons que le domaine de validité de ces approximations dépend, de la viscosité et la densité du fluide, de l'entrefer du dispositif et d'un temps caractéristique représentant la durée de la sollicitation imposée au fluide. L'influence de ces différents paramètres s'exprime par l'intermédiaire d'un nombre adimensionnel (Re) ayant la forme d'un nombre de Reynolds.

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The use of the Couette viscometer with coaxial cylinders for the evaluation of rheological properties and the establishment of behaviour laws of fluids, generally requires the knowledge of the shear rate at each instant and at any point in the gap. This quantity, which is generally unknown, can be approximated by simple mathematical expressions which are satisfactory for the applied torque flow but become less accurate as one moves away from the stationary state for the imposed speed flow. Most of the commonly used approximations are obtained under the assumption that the inertia of the fluid does not affect the flow and that the gap is small. In this work, we study the limit of the validity of certain approximations for the shear rate in an imposed speed transient flow on the example of a fluid of the Maxwell type. It is shown that the range of validity of these approximations depends on the viscosity and the density of the fluid, on the gap of the viscometer, and finally on a characteristic time representing the period under which an external perturbation is imposed to the fluid. The influence of these different parameters is expressed through a dimensionless number (Re) having the form of a Reynolds number.

     

On-line measurements of the rheological properties of fermentation broth

The paper is concerned with measurements of rheological properties of fermentation broth. An on-line rheometer, Rheohelix-1, based on the application of a helical screw impeller rotating in a draught tube has been constructed. The instrument was used for measurements of the rheological parameters of fermentation broth of Aspergillus niger in a submerged fermentation process. The results of rheological and some standard measurements have been compared and proved the applicability of the instrument.Presented at the Golden Jubilee Conference of the British Society of Rheology and Third European Rheology Conference, Edinburgh, 3–7 September, 1990.     

An anomalous phenomenon occurring in the flow of viscoelastic fluids out of ducts

When viscoelastic fluids flow out from horizontal ducts many cracks and protruding ridges are formed on the jet surface. As far as the authors know, this phenomenon has not yet been reported. The occurrence of the anomalous phenomenon is not affected by inlet flow condition or duct shape.The phenomenon may be divided into three regimes, namely, a stable state, a breakage state, and a multiplication state. In the breakage state one ridge divides into two parts after its growth, and in the multiplication state a new ridge is suddenly formed at a crack point. With increasing shear rate, the flow pattern of the jet changes from the stable state to the breakage state, and then to the multiplication state.Furthermore, a recoil effect is observed. In this effect many air bubbles rush into the duct from the exit when the flow is quickly stopped.     

Rheological properties of service weathered road bitumens

A study was carried out of the rheological properties of service weathered bitumens and their properties were compared with road performance. Bitumen from 39 test sites was recovered from the uppermost layer of stone particles covering the road surfacing and tested under dynamic and transient loading. Dynamic testing was carried out under forced sinusoidal loading. Testing under transient loading was mainly with a viscosity test conducted at 45°C, but some creep testing in compression was conducted at 0°C. From the results of dynamic testing, master curves of modulus and loss angle were constructed, spanning over ten decades in loading frequency. The hyperbolic expressions of Dickinson and Witt successfully described the frequency dependence of bitumen modulus and loss angle. The Williams, Landel and Ferry (WLF) equation, with newly derived coefficients, described the temperature dependence of the shift factor (or Newtonian viscosity) for the temperature range –10 to 60°C. Attempts were made to compare the measured transient response with that calculated from dynamic results. The result of the viscosity test conducted at 45°C as an indicator of modulus at low temperatures was assessed. Surfacing distress increased as the bitumen viscosity or modulus increased, however service performance of the bitumens was best correlated with the modulus calculated at conditions representative of traffic stressing and lowest site temperature. The changes in the rheological properties of bitumens induced by weathering is discussed.     

Quantitative evaluation of extrudate swell from viscoelastic properties of polystyrene

A theory of extrudate swell for short, intermediate or long dies is presented. In our experiment, we consider that the swelling phenomenon is mainly due to the recoverable elongational strain induced by the converging flow at the die entrance, as well as by recoverable shear strain originating within the die. From these concepts, an equation has been derived for the quantitative prediction of extrudate swell from the elastic material properties such as the entrance pressure drop, the relaxation modulus and the recoverable shear strain. Excellent agreement is found between predicted and measured values of extrudate swell obtained on commercial polystyrene melt, using capillaries of length-to-diameter ratios ranging from 1 to 20 and in a wide range of shear rates.     

Rheological properties of skim milk gels at various temperatures; interrelation between the dynamic moduli and the relaxation modulus

The rheological properties of rennet-induced skim milk gels were determined by two methods, i.e., via stress relaxation and dynamic tests. The stress relaxation modulusG _c (t) was calculated from the dynamic moduliG andG by using a simple approximation formula and by means of a more complex procedure, via calculation of the relaxation spectrum. Either calculation method gave the same results forG _c (t). The magnitude of the relaxation modulus obtained from the stress relaxation experiments was 10% to 20% lower than that calculated from the dynamic tests.Rennet-induced skim milk gels did not show an equilibrium modulus. An increase in temperature in the range from 20° to 35 °C resulted in lower moduli at a given time scale and faster relaxation. Dynamic measurements were also performed on acid-induced skim milk gels at various temperatures andG _c (t) was calculated. The moduli of the acid-induced gels were higher than those of the rennet-induced gels and a kind of permanent network seemed to exist, also at higher temperatures. G storage shear modulus,N·m^–2; - G loss shear modulus,N·m^–2; - G _c calculated storage shear modulus,N·m^–2; - G _c calculated loss shear modulus,N·m^–2; - G _e equilibrium shear modulus,N·m^–2; - G _ec calculated equilibrium shear modulus,N·m^–2; - G(t) relaxation shear modulus,N·m^–2; - G _c (t) calculated relaxation shear modulus,N·m^–2; - G ^*(t) pseudo relaxation shear modulus,N·m^–2; - H relaxation spectrum,N·m^–2; - t time,s; - relaxation time,s; - angular frequency, rad·s^–1. Partly presented at the Conference on Rheology of Food, Pharmaceutical and Biological Materials, Warwick, UK, September 13–15, 1989 [33].