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not generally longer than about 1 min, although a longer period of measurement is required to test if the criterion has been reached With much slower settling particles (either very small particles and/or a viscous liquid phase) the time to reach steady state and the measurement time may be large compared to the time it takes for a particle to settle back onto the vessel base In these situations the entire measurement is meaningless, as the system is not in equilibrium and the concentration at the base is changing with time When making visual Njs measurements, it is important to note not only the speed required to meet the chosen just suspended criterion but also the location of the point of last suspension.

All of these factors are properties of a given crystallization system, thereby requiring choices for each speci c operation. Experimentation is required to determine the key responses to mixing for each system and could include determination of the following: Effect of impeller speed and type on PSD at a minimum of two seed levels and two supersaturation ratios. These results should indicate the sensitivity of the system to mixing. A small response could indicate that other system properties were controlling (i.e., inherent crystal growth rate or nucleation rate). A large response would indicate sensitivity to secondary nucleation and/or crystal cleavage and require additional experimentation and evaluation of scale-up requirements. The laboratory results should be evaluated relative to each other since scale-up can be expected to make additional changes in PSD, especially when a large response is experienced in these simple experiments. Effect of impeller speed on crystallization rate and approach to equilibrium solubility (yield). Failure to achieve equilibrium solubility may indicate accumulation of impurities at the crystallizing surfaces. An increase in impeller speed resulting in further reduction in solution concentration could indicate resumption in growth or additional nucleation (see Example 17-3). Suspension requirements as indicated by the settling rate to achieve off-bottom suspension. The impeller speed that is found necessary to achieve off-bottom suspension should be the minimum speed on which to base scale-up, as calculated for the appropriate scale of operation. Higher speeds may be required to satisfy other requirements, as indicated below. For nucleation-dependent operations, it is recommended that additional information be obtained as follows: Effect of impeller speed on width of metastable region Effect of impeller speed and type on rate of nucleation This experimentation is focused primarily on evaluation of mixing sensitivity.

Some impeller and vessel geometry combinations tend to produce a point of last suspension in the middle of the base of the vessel; other combinations tend to leave a ring of settled solids around the base next to the vessel walls Similar visual techniques can be used to measure the equivalent speed for systems with oating particles, the just drawn-down criterion The visual observations are subject to exactly the same issues and problems as the just suspended measurements; however, access to see the particles on the free surface of the uid is generally easier to obtain than at the base of the vessel, as no transparent vessel parts are required In many situations, measurement of Njs by direct observation is impractical.

Other means must be resorted to, and two methods are available: detecting the movement of solids by means of an ultrasonic owmeter, and inferring Njs from measurements of solids concentration Both techniques are dif cult to use, and neither should be used without making visual observations in a geometrically similar vessel It is in these situations that the knowledge of the location of the last point of suspension is vital..

and ( ) S 1 1 X p (YiS a k P(Y jS b k =YiS a k ) : da;b (i; j) log2 p (YiS a k )p (Y jS b k ) S k 0

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