改进黏度在线凝胶色谱的测定结果

黏度在线凝胶色谱是一种同时配备浓度和黏度检测器的凝胶色谱，由于其测定过程简单直接，被越来越多地广泛采用，但因为数据处理方式和仪器精度的问题，其数均分子量、重均分子量与分散度结果存在较大误差．实验表明，选择适当的谱峰叠加处理、改进普适校正曲线精度、调整标样进样方式以及选择合适的积分点等手段可以明显改善存在的问题，从而大幅度地提高数均分子量、重均分子量与分散度的结果准确性。     

我国粘度计量工作中存在的问题

指出我国粘度计量工作中存在的一些问题，在修订粘度计检定规程，规范标准粘度的名称和有效期以及加强对粘度计检定工作的管理等方面的出了建议，强调了在标准粘度液证书中应给出不同温度下的运动粘度和粘度值，以满足粘度计检定工作的需要。     

Steady-state shear characteristics ofAspergillus niger broths

It can be difficult to obtain reliable rheological data for filamentous fermentation broths using conventional instruments. One common approach is to measure the torque drawn by an impeller rotating in the suspension (1–7). Many previous workers have assumed that the applicable shear rate in such a device is related to the impeller speed by a fluid-independent constant determined by calibration with Newtonian and non-Newtonian fluids (1–9). The rheology ofAspergillus niger broths have been characterized using the impeller viscometer approach. The changes in the broth rheology were measured, and used to interpret the growth of biomass and the evolution of the microorganism morphology.     

转筒黏度计测量液体黏度方法研究

用黏性流体力学理论求得测量装置中旋转液体径向速度梯度的理论公式,进而得到转筒法测量黏度的较精确公式.指出了国内的一些教材和文献在推导中使用近似公式的错误,用参数估计的方法求得测量装置的摩擦阻力力矩,使测量结果得到进一步校正.实验研究表明:按照近似公式与精确公式计算求得的径向速度梯度之差可达到13.1%,求得的液体黏度之差可达到28.6%;在蓖麻油的温度为25.5℃时测得测量装置的摩擦阻力力矩为9.482×10-5 N·m,相当于0.540克重物产生的力矩.     

Inertial contributions to the pressure in the truncated-cone-and-plate apparatus with application to dilute polymer solutions

New measurements of the pressure distribution generated by two Newtonian liquids in the Truncated Cone-and-Plate Apparatus are presented, in order to evaluate the exact form of the inertial contribution for a range of Reynolds numbers (Re) fromRe = 140 toRe = 36,000;Re = R ² /, where and are the liquid density and viscosity respectively,R is the plate radius, and is the angular velocity of the cone. The Walters equation for lowRe, p ^w = 0.15 ² (r² – R²), is shown to be in excellent agreement with the measurements up toRe = 1000, provided an appropriate correction for the Newtonian hole pressure is made. Up toRe = 1000, the measured slope is within 1% of the theoretical value of 0.15 given by the Walters equation; as the Reynolds number increases above 1000, the data become increasingly nonlinear inr ². Other theoretical predictions made especially for largeRe begin to disagree with the data even belowRe = 1000. The application of the experimentally determined additive inertial contribution to measurements of pressure distribution in four dilute polymer solutions is found to reproduce adequately the expected form of the viscoelastic pressure distribution, even at highRe where the Walters equation is not valid. Measurements of a combination of normal-stress differencesN ₁ + 2N ₂ for polymer solutions involving specific polymer/solvent interaction sites show a difference of 45% with change of solvent, while no difference is observed in solutions of polymers without the interaction sites. The normal-stress ratio —N ₂/N ₁ for a 5% solution of cis-polybutadiene is 0.24 at a shear rate of 100 s^–1, and it appears to approach the zero shear limit of 2/7 given by the Doi-Edwards theory. The Higashitani-Pritchard-Baird-Lodge equation relating the elastic hole pressure to the normal-stress differenceN ₁ –N ₂ gives a qualitative agreement betweenN ₁ –N ₂ from the TCP Apparatus and the hole pressure from the Stressmeter; the percent difference is 0 at shear stress < 25 Pa, 35% at = 45 Pa, and 18% at the highest = 63 Pa.     

DSC and Rheometry Investigations of Crude Oils

Thermal characteristics and rheological behaviour of eight crude oils covered a wide range of fluid composition and properties were studied by differential scanning calorimeter (DSC) and viscometry. Wax appearance temperatures (WAT) of crude oils were determined by DSC and viscometry. Good agreement is obtained between the results. The dynamic viscosity in the Newtonian temperature range of the crude oils (above 30°C) generally obeyed a simple first-order Arrhenius type of temperature dependence. Activation energies of flow in the non-Newtonian range are not uniquely defined. This revised version was published online in August 2006 with corrections to the Cover Date.     

Rheologische Untersuchungen an Polyacrylnitril-Spinnlösungen: Erweiterung des Viskosimeters HV 6 für höhere Temperaturen

Zusammenfassung Das Hochdruckkapillarviskosimeter HV 6 wurde für Messungen bei höheren Temperaturen adaptiert; dadurch konnten konzentrierte Lösungen von Polyacrylnitril in Dimethylformamid bis zu 120°C vermessen werden. Die erhaltenen Resultate wurden nach der Methode Vinogradov-Malkin normiert; gewisse Abweichungen, die hierbei auftraten, konnten durch Einführung eines empirischen Zusatzverschiebungsfaktors korrigiert werden.

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Summary The high pressure capillary viscometer HV 6 has been adapted for measurements at high temperatures. Concentrated solutions of polyacrylonitrile in dimethylformamide could be measured up to 120°C. The results were plotted by the Vinogradov-Malkin mastercurve method. Deviations could be corrected by introducing an empirical additional shift factor.

Mit 17 Abbildungen     

An analytical solution for the velocity and shear rate distribution of non-ideal Bingham fluids in concentric cylinder viscometers

An analytical solution is presented for the calculation of the flow field in a concentric cylinder viscometer of non-ideal Bingham-fluids, described by the Worrall-Tuliani rheological model. The obtained shear rate distribution is a function of the a priori unknown rheological parameters. It is shown that by applying an iterative procedure experimental data can be processed in order to obtain the proper shear rate correction and the four rheological parameters of the Worrall-Tuliani model as well as the yield surface radius. A comparison with Krieger's correction method is made. Rheometrical data for dense cohesive sediment suspensions have been reviewed in the light of this new method. For these suspensions velocity profiles over the gap are computed and the shear layer thicknesses were found to be comparable to visual observations. It can be concluded that at low rotation speeds the actually sheared layer is too narrow to fullfill the gap width requirement for granular suspensions and slip appears to be unavoidable, even when the material is sheared within itself. The only way to obtain meaningfull measurements in a concentric cylinder viscometer at low shear rates seems to be by increasing the radii of the viscometer. Some dimensioning criteria are presented.Notation A, B Integration constants - C Dimensionless rotation speed = µ/_y - c = 2µ - d = ₀ ²–2c_y - f() = (–₀)²+2c(–_y) - r Radius - r _b Bob radius - r _c Cup radius - r _y Yield radius - r ₀ Stationary surface radius - r Rotating Stationary radius - Y ₀ Shear rate parameter = /µ Greek letters Shear rate - = (r _y /r _b )²– 1 - µ Bingham viscosity - µ₀ Initial differential viscosity - µ µ₀-µ - Rotation speed - Angular velocity - Shear stress - _b Bob shear stress - _B Bingham stress - _y (True) yield stress - ₀ Stress parameter = _B +µ Y ₀ - _B - _y      

Shear dependence of viscosity for perfluoropolyether fluids

The shear dependence of the bulk viscosities of two structurally different types of perfluoropolyether fluids was determined by two different techniques. The first involved direct measurement in a high shear Couette viscometer, the second utilized the time-temperature superposition principle to establish master curves from viscosity determinations at low shear rates and temperature; the results are comparable. Both fluids begin to show non-Newtonian behavior at shear rates above 10,000 s^–1.