Viscosity rheometers

Piston Cylinder (Extrusion). Pressure-driven piston cylinder capillary viscometers, ie, extmsion rheometers (Fig. 25), are used primarily to measure the melt viscosity of polymers and other viscous materials (21,47,49,50). A reservoir is connected to a capillary tube, and molten polymer or another material is extmded through the capillary by means of a piston to which a constant force is appHed. Viscosity can be determined from the volumetric flow rate and the pressure drop along the capillary. The basic method and test conditions for a number of thermoplastics are described in ASTM D1238. Melt viscoelasticity can influence the results (160). 

A number of instmments are based on the extmsion principle, including sHt flow and normal capidary flow (Table 6). These instmments are useful when large numbers of quahty control or other melt viscosity test measurements are needed for batches of a single material or similar materials. When melt viscosities of a wide range of materials must be measured, rotational viscometers are preferable. Extmsion rheometers have been appHed to other materials with some success with adhesives and coatings (10,161). 

Another type of rotational viscometer is the hehcal-screw rheometer (176). This iastmment is basically a screw-type metering pump that does not pump. The measure of force is the pressure difference resulting from the rotational motion. It is possible to use a bank of pressure transducers of different sensitivities to measure viscosity over a wide range. The iastmment can be used for high temperature rheometry and to foUow polymerkation, shear and heat degradation, and other developments. 

Bohlin also markets a computer-driven controlled stress rheometer, which determines viscosity as a function of stress and measures creep and... 

The Weissenberg Rheogoniometer (49) is a complex dynamic viscometer that can measure elastic behavior as well as viscosity. It was the first rheometer designed to measure both shear and normal stresses and can be used for complete characteri2ation of viscoelastic materials. Its capabiUties include measurement of steady-state rotational shear within a viscosity range of 10 — mPa-s at shear rates of, of normal forces (elastic... 

Eig. 34. Diagram of the Rheometric Melt Elongational Rheometer (RME) for elongational viscosity measurements on polymer melts. 

Viscoelastic Measurement. A number of methods measure the various quantities that describe viscoelastic behavior. Some requite expensive commercial rheometers, others depend on custom-made research instmments, and a few requite only simple devices. Even quaHtative observations can be useful in the case of polymer melts, paints, and resins, where elasticity may indicate an inferior batch or unusable formulation. Eor example, the extmsion sweU of a material from a syringe can be observed with a microscope. The Weissenberg effect is seen in the separation of a cone and plate during viscosity measurements or the climbing of a resin up the stirrer shaft during polymerization or mixing. 

Chocolate does not behave as a tme Hquid owing to the presence of cocoa particles and the viscosity control of chocolate is quite compHcated. This non-Newtonian behavior has been described (28). When the square root of the rate of shear is plotted against the square root of shear stress for chocolate, a straight line is produced. With this Casson relationship method (29) two values are obtained, Casson viscosity and Casson yield value, which describe the flow of chocolate. The chocolate industry was slow in adopting the Casson relationship but this method now prevails over the simpler MacMichael viscometer. Instmments such as the Carri-Med Rheometer and the Brookfield and Haake Viscometers are now replacing the MacMichael. 

Specifications for soHd i7j -l,4-polyisoprenes are shown in Table 5 and include analyses for volatile matter, extractables, ash, and Mooney viscosity at 100°C. Standard method ASTM D1416 includes chemical analysis methods for volatile matter, extractables, and total ash, while ASTM D1646 includes Mooney viscosity (82). The Monsanto rheometer data for vulcanizates prepared by a standard recipe may also be specified. This formulation for vulcanizate (ASTM D3403) is mixed in a Banbury mixer in two passes with all but sulfur and accelerator added in first pass ... 

J The viscosity characteristics of a polymer melt are measured using both a capillary rheometer and a cone and plate viscometer at the same temperature. The capillary is 2.0 mm diameter and 32.0 mm long. For volumetric flow rates of 70 x 10 m /s and 200 x 10 m /s, the pressures measured just before the entry to the capillary are 3.9 MN/m and 5.7 MN/m, respectively. 

The shear viscosity, especially as measured with capillary rheometers characterized by high shear rates, is hardly sensitive to material structure since the investigator usually has to deal with the substantially destroyed structure in the molten sample. Melt stretching experiments would normally provide much more information [33]. 

FIG. 4 Viscosity (cone-plate rheometer, D = 3.23 s1, at 25°C) and clear point of 10% sodium lauryl ether (2 EO) sulfate solutions with 0.5% of added NaCl vs. percentage of dialkanolamide [77],... 

For uncompatibdized blends, the viscosity decreases with increasing number of layers in a multilayer constant stress rheometer. In the present case, the viscosity rather increases due to in situ reaction between nylon and maleated EPDM as illustrated in Figure 11.21. 

In order to test this concept a series of compounds was prepared in a 5 L Shaw Intermix (rubber internal mixer, Mark IV, Kl) with EPDM (Keltan 720 ex-DSM elastomers an amorphous EPDM containing 4.5 wt% of dicyclopentadiene and having a Mooney viscosity ML(1 +4) 125°C of 64 MU 100 phr), N550 carbon black (50 phr), diisododecyl phthalate (10 phr), stearic acid (2 phr), and l,3-bis(tert-butylperoxy-isopropyl)benzene (Perkadox 14/40 MB ex Akzo Nobel 40% active material 6 or 10 phr). A polar co-agent (15 phr) was admixed to the masterbatch on an open mill and compounds were cured for 20 min at 180°C in a rheometer (MDR2000, Alpha Technologies). The maximum torque difference obtained in the rheometer experiments was used as a measure of... 

In all of the rheometer testing of the uncured compounds, the commercial silica AZ showed the highest values with the B1 and B3 samples having the highest values among the B-series silica samples. The Mooney viscosity at 100°C increases as the number of particles in the aggregates increases. The same compounds were cured and tested, measuring tensile properties, tear resistance. 

The viscosity measurement was carried out using Brookfield Engineering Rheometer model HA DV-III equipped with small sample adapter, using spindle 28 and speed 10 rpm. Meanwhile, the melting point of the lipstick was observed with SMPI Melting Point Apparatus (Stuart Scientific). 

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