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Process optimisation (PAT-Tools)

ndustrial-scale freeze-drying requires robust processes that are initially developed on pilot systems and then scaled up. The objective is to develop drying recipes (profiles of vacuum and shelf temperature versus time) that allow the best possible quality to be achieved in the shortest possible time.

Pilot systems must therefore have the same technology and geometry as the subsequent production freeze-dryer, such as rectangular product chambers and shelves, cooled and heated by liquid media.

The following table lists the parameters used by Christ for process control and monitoring. When used together with basic recipes stored in the freeze dryer control system for various products, an automatic, self-optimising process can be achieved.

 

Feature Function Area of application Comment
dTfreezing Lowest product temperature before switching over to Freezing -> Main Drying Reliable freezing,
No defrosting or collapse of the product in entry to main drying
Preset max. permitted T-difference between product and shelf, process will adapt auto­matically
dTmain drying Lowest product temperature before switching over to the next process stage Reliable drying (main drying and final drying) Preset max. permitted T-difference between product and shelf, process will adapt auto­matically
T-sensor
wired
Product temperature measurement, traditional wired Process monitoring, determination of completion of drying Available in laboratory freeze-dryers, pilot freeze-dryers and production versions, cannot be used for automatic loading/unloading
T-sensor
wireless
WTMplus
Product temperature measurement, wireless Process monitoring, determination of completion of drying More precise, easier to position, no power input via the sensor cable
Pilot freeze-dryers and production plants
Ice condenser temperature Display and check whether desublimation is possible Onset while large amounts of steam are present and stabilisation indicates completion of drying Standard with all freeze dryers
Tshelf ON / OFF Heating fluid temperature in shelf, flow and return Difference indicates energy consumption due to sublimation Standard with
Pilot freeze-dryers and
production plants
Lyo-Rx Measurement of electrical resistance shows freezing-/melting point Determination of freezing point,
self-optimising sharp cycle possible
Freeze dryer stops heating or cooling actively on the appearance of defrosting
pPirani Drying vacuum, dependent on gas type Display of drying vacuum Traditional measurement method, typically  used in the laboratory freeze dryers
pcapacitive Drying vacuum, independent of gas type
(also known as p“MKS”)
Comparative pressure measurement More precise measurement method,
which Christ also uses in the laboratory
psafety Pre-selectable safety pressure Product protection,
Sharp cycle, limited by psafety
If specified value is exceeded (non-permitted pressure increase [=heating] of product), heating is switched off
pAlarm Pre-selectable alarm pressure Product protection,
Sharp cycle, limited by palarm
If specified value is exceeded (non-permitted pressure increase [=heating] of product), shelf cooling is activated, Pilot freeze-dryers and production plants
dp/dt
pressure increase test
Measurement of pressure increase in product chamber by closed intermediate valve Determination of final drying Continuous determination provides progressive information
dp/dt,
MTM
By measurement with rapid-closing intermediate valves, determination of T at the sublimation interface, and further thermodynamic characteristics (layer flow resistance etc.) Understanding the process, avoiding collapse

MTM = manometric temperature measurement

Pilot freeze-dryers

Dewpoint Moist gas volume Final drying of product Further information can be derived
LyoBalance Measurement of product weight during drying Final drying of product, sublimation rate Advantage of immediate measurement of the progress of drying
Pilot freeze-dryers
Camera monitoring Visual Drying quality, artefacts, faults Pilot freeze-dryers and
production plants
Controlled nucleation Uniform freezing for homogenous drying and product properties Ice fog + over-pressure method Pilot freeze-dryers and
production plants
Annealing Also referred to as tempering (crystal growth by moderate heating of the frozen product) More rapid drying without collapse,
improved structure

Laboratory freeze-dryers,
pilot freeze-dryers and
production plants

generaluse@analis.be    •    ++(0)81 25 50 50
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