An automated high-pressure,high-temperature,low-frequency viscometer

A computerized apparatus for the measurement of low shear rate viscosity on polymer solutions at elevated pressure and temperature is described. The pressure is variable from 1 bar to 400 bar with an accuracy of ±5 bar. The temperature is variable from 0° to 100°C with an accuracy of ±0.3 K. The instrument is operated in a free-relaxation mode in which the decay of oscillation of the torsion pendulum after an initial displacement is recorded and used to compute the viscosity of the sample. The measurements are performed according to the contents of a user-specified control file, and the oscillation data are stored digitally and later analyzed for parameter estimation. The instrument operates in the very-low frequency range (0.03 to 0.25 Hz) and the accuracy of the measured viscosity is ±0.03 x 10^–3 Ns/m2.     

A cryostat for use with a thermal conductivity hot wire system

Summary A cryostat for use with a thermal conductivity hot wire system is described in which temperatures between –70°C and –130°C can be maintained constant to within (0.01°C). Control of temperature is made by adjusting the vacuum between a five component mixture and liquid oxygen. Extra control is made by adjusting the current through a heating coil immersed in the cryostat mixture. The temperature indicator is a platinum wire surrounding the tubes.     

Development of temperature-compensated resistance strain gages for use to 800°C

This paper describes the development and evaluation of temperature-compensated resistance strain gages for use to 800°C. These gages included single-element gages and double-element half-bridge gages. The filament of single-element gages was fabricated from specially developed Fe–Cr–Al–V–Ti–Y alloy wire. When bonded to high-temperature Ni-based alloy GH39 after stabilization at 800°C for one hour, the apparent strain from room temperature to 800°C was less than 2000 m/m. Double-element gages were fabricated from Pt–W–Re–Ni–Cr–Y alloy wire (active grid) and Pt–Ir alloy wire (compensating grid). When bonded to different high-temperature alloy specimens and stabilized, and when ballast resistance in series with the compensating grid adjusted suitably, the gages' apparent strains from room temperature to 800°C were less than 2400 m/m.Effects of preoxidization of Fe–Cr–Al wire on the characteristics of the single-element gages are described.     

A torsional creep instrument and a torsional pendulum,both with accurate temperature control

Summary This paper describes a torsional pendulum and a torsional creep instrument. With the pendulum shear moduli between 10⁶ and 10¹⁰ N/m² can be measured at frequencies from 0.1 to 20 Hz. The creep instrument is suitable for measurement of shear compliances lower than 10^–7 m²/N in the time range from 1 to 10⁵ seconds. In both instruments, specimens are kept at the right temperature by blowing heated nitrogen gas through a surrounding thermostatic chamber. The signal of a platinum resistance thermometer, provided in each chamber, automatically controls the heating of the gas. Temperatures from –180 to +300 °C can be maintained with an absolute accuracy of ±1 °C and a long term stability of ±0.05 °C. It is shown that one cannot directly compare one and the same shear property, calculated from the shear modulus as measured with the pendulum as well as from the shear compliance as measured with the creep instrument. This is due to differences in the temperature of one thermostatic chamber over against the other. Finally, the paper presents a method to reduce these differences to ±0.1 °C, although the absolute accuracy of temperature control remains ±1 °C.

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Zusammenfassung Die Arbeit beschreibt ein Torsionspendel und eine Torsions-Kriechapparatur. Mit dem Pendel können Schermoduli zwischen 10⁶ und 10¹⁰ N/m² bei Frequenzen zwischen 0,1 und 20 °C gemessen werden. Die Kriechapparatur ist geeignet für die Messung von Scherkomplianzen kleiner als 10^–7 m²/N in Zeiten zwischen 1 bis 10⁵ sec. In beiden Geräten werden die Proben durch das Einblasen von erhitztem Stickstoff durch eine umgebende thermostatische Kammer bei der richtigen Temperatur gehalten. Die Anzeige eines Platin-Widerstandsthermometers, das in jeder Kammer angebracht ist, kontrolliert automatisch die Erwärmung des Gases. Es können Temperaturen zwischen –180 und +300 °C mit einer absoluten Genauigkeit von ±1 °C und einer Langzeitstabilität von ±0,05 °C eingestellt werden. Es wird gezeigt, daß ein direkter Vergleich der gleichen Schereigenschaft, die zum einen aus dem mit dem Pendel gemessenen Schermodul und zum anderen aus der mit der Kriechapparatur ermittelten Kriechkomplianz errechnet wird, nicht möglich ist. Das beruht auf Temperaturdifferenzen zwischen den thermostatisierten Kammern.Abschließend stellt die Arbeit eine Methode vor, um diese Differenzen auf ±0,1 °C zu senken. Die absolute Genauigkeit der Temperaturkontrolle bleibt bei ±1 °C.

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Paper presented at the Conference on Experimental Rheology, University of Bradford, April 17–19, 1968.     

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.     

The peculiar rheo-optical behavior of bisphenol A-polycarbonate and polymethylmethacrylate

The rheological and stress-optical behavior of the melts of several grades ob bisphenol-A-polycarbonate (PC) and polymethylmethacrylate (PMMA) is investigated. Pertinent flow birefringence measurements are carried out in a remodelled cone-plate apparatus [1]. The shear stress in the polymer melt is calculated from the dynamic moduli, which are determined separately. It is shown that the linear stress optical rule is obeyed. In this way, the stress-optical coefficient C of the melt can be determined. The low-Mw polycarbonates all behave as Maxwellian fluids. The main stress direction does not deviate significantly from 45°. In the temperature range from 160° to 260°C the stress-optical coefficients of the different grades lie between 3 and 4×10^–9 Pa^–1 and show a weak temperature dependence. The stress-optical coefficient of PMMA is about a factor of 100 lower and shows a peculiar temperature-dependence, changing its sign at 144°C. The results are discussed in terms of the anisotropy of the polarizability of the polymer chain.     

Can die swell be predicted?

Summary A calculational scheme has been developed to predict die swell values which are defined as the value after completion of the elastic recovery. The constants of the equations have been evaluated at 190 °C from the known results of several polyethylene samples. With the similar type but different sample of polyethylene, it is shown that the prediction is with ±3.4% for the shear rates of 90 to 600 sec^–1, for the dies ofL/D 2–20 and at temperature of 200 °C.With 3 figures and 4 tables     

A new elongational rheometer for polymer melts and other highly viscoelastic liquids

In polymer melt elongational rheometry only by the rotary clamp technique large elongations can be obtained homogeneously. However, as described in this paper, there still remain disadvantages that led to the development of a new rheometer with the following main features: The dimensions of the required sample are small (60 × 7 × 2 nun³), the sample is supported by a cushion of inert gas and, after having reached the test temperature of up to well above 300°C, it can be extended by a new type of clamps that make use of metal conveyor belts. The resulting tensile force is measured with a resolution of better than 100 mgf (0.001 N). The strain rate range is 0.001-1 s^–1, and the maximum Hencky strain is 7, corresponding to a maximum stretch ratio of 1100. Within the sample, the temperature variation in time and space is less than 0.1°C. For the evaluation and documentation of the test performance, a video camera records the top and side views of the sample that carries a marking powder to permit the evaluation of the true strain rate. The operation of the instrument is easy, and so is the sample preparation, but care must be taken concerning the necessary isotropy and internal homogeneity. Examples of test results are given for several polymer melts at various temperatures: (1) Polystyrene up to a total Hencky strain larger than 7 at 170°C, (2) several types of polyethylene (LDPE, LLDPE, HDPE) at 150°C, (3) poly(amide) at 250°C, and (4) poly(ethersulfone) at 350°C. The wide applicability of the new rheometer is demonstrated by adding results obtained from samples of bread dough. The surface tension has no influence on the results if an error of 3% can be tolerated. From the results it follows that by means of the newly developed rheometer many problems in polymer melt elongation have been solved.Dedicated to Professor Dr. Hermann Janeschitz-Kriegl on the occasion of his 70th birthday.Extended version of a paper presented at the XIth International Congress on Rheology, Brussels, Belgium, August 17–21, 1992.     

Direct measurement of static yield properties of cohesive suspensions

A technique of yield stress investigation based upon the combined use of two devices (an applied stress rheometer and an instrument for measuring the propagation velocity of small amplitude, torsional shear waves) is described. Investigations into the low shear rate rheological properties of illitic suspensions are reported for shear rates, typically, in the range 10^–4— 10^–1 s^–1 under applied stresses in the range 0.01 — 10 Nm^–2 and involving shear strains between 10^–1 and 10^–4. Results are presented which demonstrate that the technique does not invoke the excessive structural disruption of material associated with applied shear rate based methods (direct and otherwise) and the widely encountered problem of wall slip at the surface of rotational measuring devices is avoided using miniature vane geometries. Results are compared with those obtained using smooth-walled cyclindrical measuring devices in both applied stress and applied shear rate instruments.Yield measurements are considered in relation to the structural properties of the undisturbed material state and shear moduli obtained by studying the propagation of small amplitude (10^–5 rad), high frequency (~ 300 Hz) torsional shear waves through the test materials are reported. Experimental techniques and instrument modifications to permit these measurements are described.     

Messung der Wärmeleitfähigkeit flüssiger Benzolderivate mit einem instationären Hitzdrahtverfahren

Zusammenfassung Im Temperaturbereich von –85 °C bis +275 °C wurde mit einer Relativmethode die Wärmeleitfähigkeit von 32 flüssigen Benzolderivaten, nämlich von Benzol, Naphthalin, Anthracen, Phenanthren, Pyren, 13 Halogenbenzolen (darunter 10 Chlorbenzole), 9 Methylbenzole und 5n-Alkylbenzole, gemessen.

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Liquid thermal conductivities of derivatives of benzene measured by an unsteady state hot wire method

In the temperature range between –85 °C and +275 °C the liquid thermal conductivity of 32 derivatives of benzene, namely of benzene, naphthalene, anthracene, phenanthrene, pyrene, 13 halogenated benzenes (10 chloro benzenes), 9 methylbenzenes and 5n-alkylbenzenes was measured by an unsteady state hot wire method.

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Herrn Prof. Dr.P. Grassmann möchte ich für seine vielen Ratschläge und Hinweise meinen besten Dank aussprechen. Ebenso gilt mein Dank dem Eidg. Volkswirtschaftsdepartement, das diese Arbeit aus dem Arbeitsbeschaffungskredit des Bundes finanzierte.     

Dynamic instabilities of boiling two-phase flow in a single horizontal channel

Dynamic instabilities of two-phase flow associated with refrigerant R-11 in a uniformly heated horizontal in-tube boiling system were experimentally investigated. An experimental setup was designed and built to work in a wide range of mass fluxes G [75–1050 kg/(m² s)], heat fluxes q (0–100 kW/m²), and fluid inlet temperatures T_inlet (2–24°C). Dynamic instability data were obtained under various working conditions. The dependence of oscillation amplitude and period on system parameters is discussed, and the boundaries of various oscillations are located on the steady-state characteristic curves.     

High-temperature pressure-shear plate impact experiments using pure tungsten carbide impactors

The pressure-shear plate impact experiment has been modified to test materials at high temperatures (up to 700°C). Together with the high strain rates characteristic of this experiment (10⁶ s^–1), the high-temperature capability allows the shearing resistance of materials to be measured under conditions unattainable with other testing equipment. The compressive and shear responses of pure tungsten carbide at different temperatures are presented, as well as the results of one test on OFHC copper at a temperature of 691°C and a shear strain rate of 1.4×10⁶ s^–1.     

A new transient method for analysis of solidification in the continuous casting of metals

Solidification processes involve complex heat and mass transfer phenomena, the modelling of which requires state-of-the art numerical techniques. An efficient and accurate transient numerical method is proposed for the analysis of phase change problems. This method combines both the enthalpy and the enhanced specific heat approaches in incorporating the effects of latent heat released due to phase change. The sensitivity and accuracy of the proposed method to both temporal and spatial discretization is shown together with closed-form solutions and the results from the enhanced specific heat approach. In order to explore the proposed method fully, a non-linear heat release, as is the case for binary alloys, is also examined. The number of operations required for the new transient approach is less than or equal to the enhanced heat capacity method depending on the averaging method adopted. To demonstrate the potential of this new finite-element technique, measurements obtained on operating machines for the casting of zinc, aluminum and steel are compared with the model predictions. The death/birth technique, together with the proper heat-transfer coefficients, were employed in order to model the casting process with minimal error due to the modelling itself.Nomenclature [A] conductance matrix - [B] matrix containing the derivative of the element shape functions - c, C _p specific heat (J kg^–1°C^–1) - effective specific heat (J kg^–1°C^–1) - f(T) local liquid fraction - f thermal load vector - H enthalpy (J kg^–1) - [H] capacitance matrix - h, h _r,h _c heat transfer coefficient (W m^–2°C^–1) - K thermal conductivity (W m^–1°C^–1) - L latent heat of solidification (J kg^–1) - l overall length (m) - N _i shape functions - Q rate of heat generation per unit volume (J m^–3) - q heat flux (W m^–2) - R residual temperature (°C) - T temperature (°C) - T _s solidus temperature (°C) - T _l liquidus temperature (°C) - T _pouring pouring temperature (°C) - T _top temperature at the top of the mould (°C) - T _w temperature of the water spray (°C) - approximated temperature (°C) - T surrounding temperature (°C) - cooling rate (°C/s) - t time (seconds) - x _i,x, y, z spatial variables (m) - t time step (s) - x element size (m) - diffusivity (m²s^–1) - density (kg m^–3) - time marching parameter - _n direction cosines of the unit outward normal to the boundary     

Ein vollautomatisch arbeitendes Torsionspendel für den Temperaturbereich von −180°C bis + 250°C

Zusammenfassung Zur Ermittlung des komplexen SchubmodulsG ^* bei Kunststoffen wurde ein Torsionspendel an einen Prozeßrechner angeschlossen. Das Meßsystem gestattet es, Messungen in einem Temperaturbereich von –180°C bis +250°C bei einer konstanten Schwingungsfrequenz von 1 Hz ± 0,09 Hz vollautomatisch durchzuführen. Der Rechner hat die Aufgabe, das Experiment zu steuern, die Versuchsbedingungen zu kontrollieren, die Meßwerte zu erfassen und die Auswertung durchzuführen. Die Ergebnisse können in Form von Tabellen oder graphisch ausgegeben werden. Ferner ist es möglich, die Ergebnisse auf dem Massenspeicher des Rechners in einer Datei abzulegen.

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Summary A torsional pendulum has been connected to a minicomputer in order to measure the complex shear modulus (G ^*). This experimental set-up allows to take computer controlled measurements in the temperaturerange –180°C to +250°C at a constant oscillation frequency of 1 Hz ± 0,09 Hz. The setting and controlling of the experimental parameters, the take-up of the data and the calculations are performed by the computer. The results are obtained in tabulated form or in form of plotted diagrams. In addition it is possible to store the results on the disc of the computer.

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Mit 10 Abbildungen     

Exergy efficiency of a counterflow air/air heat exchanger with vapour condensation

The exergy efficiency of a counterflow hot moist air/ambient air heat exchanger with vapour condensation as a function of the temperature and humidity of the hot moist air, the ratio of ambient air flow rate to hot moist air flow rate and the minimum temperature differences between the flows is determined. The ranges 20 to 120°C and 0.01 to 1.0 kg·kg^–1 for the temperature and humidity ratio of hot moist air respectively are considered. Constant ambient air conditions of 20°C and 0.01 kg·kg^–1 were assumed.

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Exergie-Wirkungsgrad eines Luft/Luft-Gegenstrom-Wärmetauschers mit Dampfkondensation

Zusammenfassung Der Exergie-Wirkungsgrad eines Gegenstrom-Wärmetauschers wird bestimmt für die Kombination: heiße Feuchtluft zu Umgebungsluft mit Dampfkondensation, und zwar als Funktion von Temperatur und Feuchtegrad der heißen Feuchtluft, des Verhältnisses von Umgebungsluft zu heißen Feuchtluftstrom und der minimalen Temperaturdifferenz zwischen beiden Strömen. Die Temperatur des heißen Feuchtluftstroms variiert im Bereich von 20 bis 120°C, sein Feuchtegrad im Bereich 0,01 bis 1,0. Bezüglich der Umgebungsluft wurden konstante Bedingungen angenommen, und zwar 20°C und ein Feuchtegrad von 0,01.

     

Elevated temperature testing with the torsional split hopkinson bar

The torsional split-Hopkinson-bar technique is modified for high-strain-rate testing at elevated temperatures by heating the specimen rapidly and keeping the rest of the apparatus at room temperature. Tests have been conducted with specimens made of several materials (Haynes-188, 1020 steel, and 1151 steel) at temperatures ranging from 650°C to 1060°C and strain rates on the order of 1000 s^–1.     

Comportement rheologique de sols d'acide polysilicique. II. Etude de la gélification

Résumé L'analyse du comportement rhéologique de sols d'acide polysilicique en solution aqueuse de concentration supérieure à 7 g 1^–1 de silice en fonction du pH entre 6 et 11 et de la température entre 25 et 45 °C a permis de situer la gélification dans un domaine de pH compris entre 8 et 10. Ce processus prend une intensité maximale à 30°C. Le comportement rhéofluidifiant à bas gradients de cisaillement et antithixotrope donne naissance sur les rhéogrammes à un point d'inversion à pH = 9. L'ionisation des groupes silanols à la surface des particules colloïdales permet la réorganisation du milieu après cisaillement. Un état d'ionisation trop élevé est responsable d'un effet electro-répulsif à pH = 10. L'influence de la concentration et de la température sur ces processus est discutée.

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The rheological behavior of polysilicic acid in aqueous solutions at higher concentrations than 7 g 1^–1 of silice is studied for pH between 6 and 11 with temperature varying from 25° to 45°C. This study indicates that gelification takes place between pH 8 and 10. The process of gel formation attains the highest intensity at 30°C. The shear-thinning behavior at low shear rate gives rise to an inversion point at pH = 9 in shear stress—shear rate curves. The state of ionization at the surface of colloïdal silice particles after shear involve shear thickening observed at pH = 9. A high ionization degree causes an electrostatic repulsion at pH = 10. The concentration and temperature effects upon the organization of network are discussed.

     

Heat Transport in Unsaturated Zone Thermal Energy Storage – Analysis with Two-Phase and Single-Phase Models

We analyze a field experiment where ambient air is injected into the soil during the summer and extracted again during the winter. A multiphase model accounting for the conductive transport as well as the convective transport with the moving liquid and gas phases is used along with a more simplified single-phase model where the convective transport is due to the gas alone. The latter model also accounts for subzero wintertime temperatures. The multiphase model captures well both the seasonal variations and the actual test sequence, the main calibration being in the adjustment of medium permeabilities based on the observed pressure responses. The effect of the injection pump on the temperature and humidity of the injection air needs to be known accurately. Taking into account the humidity of the injection air explicitly instead of using humidity-corrected enthalpy values also has an effect. The effect of various humidity and specific enthalpy assumptions is of the order of 1–1.5°C, while ignoring the wintertime subzero temperatures has an effect of 1–2°C. These differences are of the same order of magnitude as the heterogeneity-introduced differences in field data. Using the simplified single-phase model typically appears to cause a difference of 1–2°C, but can yield an even higher deviation of the order of 3–4°C.     

Superheating instability in a pulsed xenon discharge

It is shown that previously obtained conditions for superheating instability substantially vary if we take into account secondary xenon ionization. Instability completely vanishes if the density of heavy particles in the discharge is kept constant and whenever a discontinuous time variation of temperature T in a restricted region between 15 · 10³ ° K and 20 · 10³ ° K is possible for a constant effective pressure. The development of instability is studied numerically by a ranging method. Stationary temperature distributions possessing a high contrast as a local temperature passes through a given range of instability with constant pressure are presented.Translated from Zhurnal Prikladnoi Mekhaniki i Tekhnicheskoi Fiziki, No. 1, pp. 27–30, January–February, 1976.     

An improved Couette high shear viscometer

Summary The advantages of theCouette-type concentric cylinder viscometer have been cited for making viscosity measurements at high shear rates. Significant improvements in theBarber design are described which have resulted in the development of an instrument which can make measurements under laminar shear conditions at over several decades of shear rate. The range is over twice that of previous instruments demonstrating the achievement of shear rates to above 1 000 000 sec^–1, and with minimum viscous heating and over a temperature range of over 100°C.

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Zusammenfassung Nachdem auf die Vorteile desCouette-Viskosimeters für Viskositätsmessungen bei hohen Schergeschwindigkeiten hingewiesen worden ist, werden wesentliche Verbesserungen des Geräts nachBarber beschrieben, die zur Entwicklung eines Instruments geführt haben, das Messungen unter laminaren Scherbedingungen über mehrere Dekaden der Schergeschwindigkeit erlaubt. Der Bereich ist mehr als doppelt so groß wie bei früher beschriebenen Instrumenten und reicht bis über 10⁶ sec^–1. Dabei tritt nur eine geringe viskose Erwärmung auf, und es kann noch bei Temperaturen von mehr als 100°C gemessen werden.

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With 4 figures and 2 tables