Viscosity instrumentation

Certain calibrated orifice instruments (Engler-type) provide viscosity measurements at temperature lower than pour point. This is possible because the apparatus agitates the material to the point where large crystals are prevented from forming whereas in other methods, the sample pour point is measured without agitation. 

The concentric cylinder viscometer described in Sec. 2.3, as well as numerous other possible instruments, can also be used to measure solution viscosity. The apparatus shown in Fig. 9.6 and its variations are the most widely used for this purpose, however. One limitation of this method is the fact that the velocity gradient is not constant, but varies with r in this type of instrument, as noted in connection with Eq. (9.26). Since we are not considering shear-dependent viscosity in this chapter, we shall ignore this limitation. 

The temperature must be raised when there is no solvent that can dissolve samples at ambient temperature. For example, polyolefines such as polyethylene and polypropylene are usually analyzed at 130-140°C because no solvent can dissolve these polyolefines at lower temperatures. It is also preferable to perform analyses at elevated temperatures when the viscosity of the elution solvent is considerably higher at ambient temperature. However, a temperature around 25-40°C is recommended when good solvents having low viscosity are available at such a temperature. It is much more convenient to operate a GPC instrument at 25-40°C than to operate at higher temperatures. 

Direct Indicating Viscometer. This is a rotational type instrument powered by an electric motor or by a hand crank. Mud is contained in the annular space between two cylinders. The outer cylinder or rotor sleeve is driven at a constant rotational velocity its rotation in the mud produces a torque on the inner cylinder or bob. A torsion spring restrains the movement. A dial attached to the bob indicates its displacement. Instrument constants have been so adjusted that plastic viscosity, apparent viscosity, and yield point are obtained by using readings from rotor sleeve speeds of 300 and 600 rpm. 

Other properties of solvents which need to be considered are boiling point, viscosity (lower viscosity generally gives greater chromatographic efficiency), detector compatibility, flammability, and toxicity. Many of the common solvents used in HPLC are flammable and some are toxic and it is therefore advisable for HPLC instrumentation to be used in a well-ventilated laboratory, if possible under an extraction duct or hood. 

The most widely used molecular weight characterization method has been GPC, which separates compounds based on hydrodynamic volume. State-of-the-art GPC instruments are equipped with a concentration detector (e.g., differential refractometer, UV, and/or IR) in combination with viscosity or light scattering. A viscosity detector provides in-line solution viscosity data at each elution volume, which in combination with a concentration measurement can be converted to specific viscosity. Since the polymer concentration at each elution volume is quite dilute, the specific viscosity is considered a reasonable approximation for the dilute solution s intrinsic viscosity. The plot of log[r]]M versus elution volume (where [) ] is the intrinsic viscosity) provides a universal calibration curve from which absolute molecular weights of a variety of polymers can be obtained. Unfortunately, many reported analyses for phenolic oligomers and resins are simply based on polystyrene standards and only provide relative molecular weights instead of absolute numbers. 

Uncoupled Rate Constants. An initial evaluation of polymerization kinetics is presented in Figure (2), constrained by viscosity invariant rate constants K. The slopes of these straight lines give initial estimates of Rgg/Kp according to Equation (14). Figure 3 presents graphically a power law relationship between K g/Kp and viscosity at 21°C and at 16.6 C. More scatter In Yu s data may be attributed to the use of an older GPC instrument of relatively low resolution. The ratio Kgq/Kp is temperature-sensitive a change of the order or five times is observed if the temperature is reduced by 4.4°C and viscosity is kept constant. 

As a major branch of nanotribology. Thin Film Lubrication (TFL) has drawn great concerns. The lubricant him of TFL, which exists in ultra precision instruments or machines, usually ranges from a few to tens of nanometres thick under the condition of point or line contacts with heavy load, high temperature, low speed, and low viscosity lubricant. One of the problems of TFL study is to measure the him thickness quickly and accurately. The optical method for measuring the lubricant him thickness has been widely used for many years. Goher and Cameron [3] successfully used the technique of interferometry to measure elastohydrody-namic lubrication him in the range from 100 nm to 1 /rm in 1967. Now the optical interference method and Frustrated Total Reflection (FTR) technique can measure the him thickness of nm order. 

Melvin Mooney devised an instrument to measure the stiffness of uncured compounds, also known as the compound s viscosity. The unit of measurement is expressed in Mooney units. Figure 28.1 shows an instrument set up for measuring viscosity, the Mooney viscometer, in which a knurled knob (rotor) rotates (at 2 revolutions per minute) in a closed heated cavity filled with rubber [2]. 

A series of calibration standards (CS) is made up that covers the concentration range from just above the limit of detection to beyond the highest concentration that must be expected (extrapolation is not accepted). The standards are made up to resemble the real samples as closely as possible (solvent, key components that modify viscosity, osmolality, etc.). A series of blinded standards is made up (usually low, medium, high the analyst and whoever evaluates the raw data should not know the concentration). Aliquots are frozen in sufficient numbers so that whenever the method is again used (later in time, on a different instrument or by another operator, in another laboratory, etc.), there is a measure of control over whether the method works as intended or not. These so-called QC-standards (QCS) must contain appropriate concentrations of all components that are to be quantified (main component, e.g., drug, and any impurities or metabolites). 

Natural ingredients based lipstick formulations have been prepared. The effects of the natural waxes, oils and solvent compositions on the viscosity and melting point of the lipstick have been studied. The result indicates that the viscosity and melting point of the lipstick can be manipulated by changing the composition of natural candelilla wax, camauba wax and beeswax in the formulation. Another important lipstick characteristic, which is hardness, will be studied. Consumer acceptance towards the product will be investigated. Finally, by relating the consumer data and instrumentation analysis, optimisation process will be conducted. 

In the pneumatic pumping system, the pressure (and not the flow rate) is maintained constant as variations in chromatographic conditions occur. Thus, a change in mobile phase viscosity (e.g. gradient elution) or column back pressure will result in a change in flow rate for these types of pumps. The gas displacement pump in which a solvent is delivered to the column by gas pressure is an example of such a pneumatic pump. The gas displacement system is among the least expensive pumps available and is found in several low cost instruments. While the pump is nonpulsating and hence, produces low noise levels with the detectors in current use, its flow stability and reproducibility are only adequate. In addition, its upper pressure limit is only 2000 psi which may be too low in certain applications. 

Historically, viscosity measurements have been the single most important method to characterize fluids in petroleum-producing applications. Whereas the ability to measure a fluid s resistance to flow has been available in the laboratory for a long time, a need to measure the fluid properties at the well site has prompted the development of more portable and less sophisticated viscosity-measuring devices [1395]. These instruments must be durable and simple enough to be used by persons with a wide range of technical skills. As a result, the Marsh funnel and the Fann concentric cylinder, both variable-speed viscometers, have found wide use. In some instances, the Brookfield viscometer has also been used. 

Reciprocating-piston pumps deliver a constant flow at si fixed backpressure. At high pressures some minor flow variability ziay arise due to the compressibility of the mobile phase. Soms instruments incorporate a flow controller which provides a fixadi backpressure for the pump to work against, independent of the column backpressure. The influence of pressure fluctuations, solvent compressibility, and solvent viscosity on the volumetrie output of the pump are thereby eliminated. Reciprocating-piston pumps can provide continuous solvent delivery, fast solvent change--... 

When using any solvent extraction system, one of the most important decisions is the selection of the solvent to be used. The properties which should be considered when choosing the appropriate solvent are selectivity distribution coefficients insolubility recoverability density interfacial tension chemical reactivity viscosity vapour pressure freezing point safety and cost. A balance must be obtained between the efficiency of extraction (the yield), the stability of the additive under the extraction conditions, the (instrumental and analyst) time required and cost of the equipment. Once extracted the functionality is lost and... 

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