Viscometer, capillary

Cm.OROCARBONSANDCm.OROHYDROCARBONS - RDIG-Cm.ORINATED TOLUENES] (Vol 6) Piston cylinder capillary viscometer... 

Dilute Polymer Solutions. The measurement of dilute solution viscosities of polymers is widely used for polymer characterization. Very low concentrations reduce intermolecular interactions and allow measurement of polymer—solvent interactions. These measurements ate usually made in capillary viscometers, some of which have provisions for direct dilution of the polymer solution. The key viscosity parameter for polymer characterization is the limiting viscosity number or intrinsic viscosity, [Tj]. It is calculated by extrapolation of the viscosity number (reduced viscosity) or the logarithmic viscosity number (inherent viscosity) to zero concentration. 

The viscosity ratio or relative viscosity, Tj p is the ratio of the viscosity of the polymer solution to the viscosity of the pure solvent. In capillary viscometer measurements, the relative viscosity (dimensionless) is the ratio of the flow time for the solution t to the flow time for the solvent /q (Table 2). The specific (sp) viscosity (dimensionless) is also defined in Table 2, as is the viscosity number or reduced (red) viscosity, which has the units of cubic meters per kilogram (m /kg) or deciUters per gram (dL/g). The logarithmic viscosity number or inherent (inh) viscosity likewise has the units m /kg or dL/g. For Tj g and Tj p, the concentration of polymer, is expressed in convenient units, traditionally g/100 cm but kg/m in SI units. The viscosity number and logarithmic viscosity number vary with concentration, but each can be extrapolated (Fig. 9) to zero concentration to give the limiting viscosity number (intrinsic viscosity) (Table 2). 

Fig. 12. Viscosity at different temperatures measured by a capillary viscometer injection-molding grade of poly(methyl methacrylate) (43). To convert N/m to psi, multiply by 145 to convert (N-s)/m to (dyn-s)/cm (P), multiply by 10.

Capillary Viscometers. Capillary flow measurement is a popular method for measuring viscosity (21,145,146) it is also the oldest. A Hquid drains or is forced through a fine-bore tube, and the viscosity is determined from the measured flow, appHed pressure, and tube dimensions. The basic equation is the Hagen-Poiseuike expression (eq. 17), where Tj is the viscosity, r the radius of the capillary, /S.p the pressure drop through the capillary, IV the volume of hquid that flows in time /, and U the length of the capillary. 

Capillary viscometers are useful for measuring precise viscosities of a large number of fluids, ranging from dilute polymer solutions to polymer melts. Shear rates vary widely and depend on the instmments and the Hquid being studied. The shear rate at the capillary wall for a Newtonian fluid may be calculated from equation 18, where Q is the volumetric flow rate and r the radius of the capillary the shear stress at the wall is = r Ap/2L. 

Absolute viscosities are difficult to measure with capillary viscometers, but viscosities relative to some standard fluid of known viscosity, such as water, are readily determined. The viscometer is caHbrated with the reference fluid, and viscosities of other fluids relative to the reference sample are determined from their flow times. 

Gla.ss Ca.pilla.ry Viscometers. The glass capillary viscometer is widely used to measure the viscosity of Newtonian fluids. The driving force is usually the hydrostatic head of the test Hquid. Kinematic viscosity is measured directly, and most of the viscometers are limited to low viscosity fluids, ca 0.4—16,000 mm /s. However, external pressure can be appHed to many glass viscometers to increase the range of measurement and enable the study of non-Newtonian behavior. Glass capillary viscometers are low shear stress instmments 1—15 Pa or 10—150 dyn/cm if operated by gravity only. The rate of shear can be as high as 20,000 based on a 200—800 s efflux time. 

Fig. 24. (a) Ostwald glass capillary viscometer, (b) Cannon-Fenske viscometer, and (c) Ubbelohde viscometer. 

AH glass capillary viscometers should be caUbrated carefully (21). The standard method is to determine the efflux time of distilled water at 20°C. Unfortunately, because of its low viscosity, water can be used only to standardize small capillary instmments. However, a caUbrated viscometer can be used to determine the viscosity of a higher viscosity Hquid, such as a mineral oil. This oil can then be used to caUbrate a viscometer with a larger capillary. Another method is to caUbrate directly with two or more certified standard oils differing in viscosity by a factor of approximately five. Such oils are useful for cahbrating virtually all types of viscometers. Because viscosity is temperature-dependent, particularly in the case of standard oils, temperature control must be extremely good for accurate caUbration. 

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). 

Melt Index Tester MTS Capillary Viscometer Automatic Capillary Rheometer ProcessibiLity Tester... 

A number of viscometers have been developed for securing viscosity data at temperatures as low as 0 °C (58,59). The most popular instmments in current use are the cone plate (ASTM D3205), parallel plate, and capillary instmments (ASTM D2171 and ASTM D2170). The cone plate can be used for the deterniination of viscosities in the range of 10 to over 10 Pa-s (10 P) at temperatures of 0—70°C and at shear rates from 10 to 10 5 . Capillary viscometers are commonly used for the deterniination of viscosities at 60 —135°C. 

Capillary viscometers are simple and inexpensive. They are normally constructed from glass and resemble a U-tube with a capillary section between two bulbs. The initial design originated with Ostwald and is shown as part A in Figure 3.2-1. The Cannon-Fenske type, a popular modification of the Ostwald design that moves the bulbs into the same vertical axis, is shown as part B in Figure 3.2-1. 

Figure 3.2-1 Diagrams of (A) Ostwald and (B) Cannon-Fenske capillary viscometers.

I = complex impedance, B = conductivity bridge, C = capillary viscometer, P = pycnometer or dilatometer, V = volumetric glassware, I = instrument, U = method unknown... 

Rheological and processability behaviors were studied in a Monsanto processability tester (MPT), which is an automatic high-pressure capillary viscometer. The entire barrel and capillary are electrically heated with a microprocessor-based temperature controller [14], The... 

Experiments with a capillary viscometer of length 100 mm and diameter 2 mm gave the following results ... 

In practice we do not measure viscosity directly. Instead, what is measured is time of flow for solutions and pure solvent in a capillary viscometer, the so-called efflux time. If the same average hydrostatic head is used in all cases, and since for very dilute solutions the density differences between the different concentrations are negligible, then the ratio of the efflux time of the solution, t, to that of the pure solvent, tg, may be taken as a measure of the ratio of the viscosities, i.e. 

The viscosities of aqueous solutions of PGA were determined with an Ubbelhode capillary viscometer at 298 K in the same concentration range as the density measurements. The temperature of the water bath was maintained to 0.05K. 

The specific viscosity Tj for different values of the concentration (C) of the analyzed polysaccharide solutions in 0.15 M NaCl was determined by means of a capillary viscometer (Ubbelode) at 25°C. 

The experimental procedure employed a capillary viscometer made of quartz as shown in Fig. 26. A solid sample was put in the filtration chamber and the top of the chamber was sealed under a vacuum. Then the sample was heated to melting and filtered into the viscometer and the connecting tube sealed at the middle. The viscometer was settled inside a transparent electric furnace and after the temperature of the melt was stabilized, the furnace containing the viscometer was turned upside down, which transferred the melt into the funnel. Then the tube was turned... 

Figure 26. Capillary viscometer. (Reprinted from Ref. 135 with permission of the Chemical Society of Japan.)...

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