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FRESH PERSPECTIVES


Figure 7 - Cycle after controlled nucleation using FreezeBooster technology. The primary drying time was reduced to 30 hours.


The combination of controlled nucleation with controlled heat fl ow during freezing resulted in lower product temperatures during primary drying due to lower cake resistance, thus allowing the shelf temperature to be increased and shorter primary drying times achieved.


Another powerful feature of measuring the heat fl ow is that the End of Primary Drying can be detected. As can be seen in Figures 9 and 10, the heat fl ux measurement was in direct agreement with the pressure


Figure 9 - Primary drying post-controlled nucleation and AccuFlux ice crystal growth control, shelf temperature was raised to -12°C. A 46.3% reduction in primary drying time.


Figure 8 - Cycle with controlled nucleation using FreezeBooster and then AccuFlux was used to control the crystal growth at an arbitrary level. The primary drying time was reduced to 28 hours. It is very important to note that the product temperature ran at 4° to 5°C lower. AccuFlux produced an ice crystal structure that had a far lower cake resistance.


Figure 10 - Further reduction in primary drying time using AccuFlux to control the shelf temperature based on the product temperature, which was calculated using the heat fl ux data. The result is a 53% reduction in overall primary drying time.


The ability to monitor and control the freezing process enables the operator to develop a fully controllable and repeatable ice and cake structure. Further testing and fi eld results will provide more information on the best heat fl ow control levels and profi les during freezing to produce the best pore structure and lowest cake resistance for a specifi c product. If desired, controlling the heat fl ow can also be used to produce a consistent collapsed structure as well.


73 American Pharmaceutical Review | Fresh Perspectives 2013


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