Mechanical property measurement procedure

Tablet mechanical properties measured on samples prepared on an instrumented tablet press or compaction simulator are an excellent means to characterize excipients under dynamic conditions (8,9). Meaningful data analyses are best achieved if both tablet preparation and tablet property measurements are performed at carefully controlled conditions using standardized procedures. Such testing in the authors ...

This procedure produced clear stable membranes with reproducible mechanical properties independent of past history of the film. Extmded films, solvent cast films, and uniaxially stressed films with different thickness were all converted to isotropic films with identical elastic modulus and water uptake response after this protocol. We wDl present results of mechanical property measurements that show why the specifics of this protocol are important. The key to reproducibility, as we shall show, is to remove aU structure associated with clustering of the sulfonic acid groups in the polymer. 

The Institute has many-year experience of investigations and developments in the field of NDT. These are, mainly, developments which allowed creation of a series of eddy current flaw detectors for various applications. The Institute has traditionally studied the physico-mechanical properties of materials, their stressed-strained state, fracture mechanics and developed on this basis the procedures and instruments which measure the properties and predict the behaviour of materials. Quite important are also developments of technologies and equipment for control of thickness and adhesion of thin protective coatings on various bases, corrosion control of underground pipelines by indirect method, acoustic emission control of hydrogen and corrosion cracking in structural materials, etc. 

The procedures of measuring changes in some physical or mechanical property as a sample is heated, or alternatively as it is held at constant temperature, constitute the family of thermoanalytical methods of characterisation. A partial list of these procedures is differential thermal analysis, differential scanning calorimetry, dilatometry, thermogravimetry. A detailed overview of these and several related techniques is by Gallagher (1992). 

The measurement of mechanical properties is a major part of the domain of characterisation. The tensile test is the key procedure, and this in turn is linked with the various tests to measure fracture toughness... crudely speaking, the capacity to withstand the weakening effects of defects. Elaborate test procedures have been developed to examine resistance to high-speed impact of projectiles, a property of civil (birdstrike on aircraft) as well as military importance. Another kind of lest is needed to measure the elastic moduli in different directions of an anisotropic crystal this is, for instance, vital for the proper exploitation of quartz crystal slices in quartz watches. 

Additional suggested resources for the reader include introductory articles on scanning probe techniques for materials properties measurement [82,83J. A comprehensive manual describing various surface preparation techniques, experimental procedures and instrumentation is also a good resource [84J, although the more recent modulation based techniques are not covered. Key textbooks include Johnson s on contact mechanics [51J and Israelachvili s on surface forces [18J, as well as a treatment of JKR/DMT issues by Maugis [85J. 

Very recently, Williams, Billington Pearson (1992) have examined the effect of reinforcement by silver or silver-tin alloy on the mechanical properties of three glass-ionomer cements. Measurements of compressive, flexural, tensile (measured by the diametral compressive procedure) and shell strength are given in Table 5.17. These results show that the effect of reinforcement varies from cement to cement but, in general, increases it. 

Powder flow is most frequently thought of as relevant to formulation development, and there are numerous references attempting to correlate any one of a number of measures of powder flow to the manufacturing properties of a formulation [34—40]. In particular, the importance of physical properties in affecting powder flow has been well documented. Research into the effect of the mechanical properties on powder flow has, however, been very limited. It is, of course, important to be able to determine and quantitate the powder flow properties of formulations. It is of equal importance, however, to determine the powder flow characteristics of bulk drug early in the development process (preformulation phase). Often, the preformulation or formulation scientist is constrained by time, materials, and manpower. Yet certainly the preformulation studies carried out should be meaningful. Well-defined experimental methods and procedures should be used the information generated should be reproducible and permit useful predictions to be made. 

A final comment seems to be pertinent. In most cases actual measurements are not made at the frequencies of interest. However, one can estimate the corresponding property at the desired frequency by using the time (fre-quency)-temperature superposition techniques of extrapolation. When different apparatuses are used to measure dynamic mechanical properties, we note that the final comparison depends not only on the instrument but also on how the data are analyzed. This implies that shifting procedures must be carried out in a consistent manner to avoid inaccuracies in the master curves. In particular, the shape of the adjacent curves at different frequencies must match exactly, and the shift factor must be the same for all the viscoelastic functions. Kramers-Kronig relationships provide a useful tool for checking the consistency of the results obtained. 

Mechanical properties of parts were determined using standard ASTM procedures. Beat sag measurements reflect the verticle drop in inches of a four inch cantilevered specimen after exposure to a given temperature for a given length of time. 

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