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Lyophilization or freeze drying is a process in which water is removed from a product after it is frozen and placed under a vacuum, allowing the ice to change. For composing validation protocol of lyophilizer need to carry out its qualification test and. decide acceptance criteria. So during selection of. Hi all, I have a question regarding an OQ of a freeze dryer. Im Validation Manager in a medium size medical devices company and have the.

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Validation Equipment – Lyophilizer Qualifications

The vacuum system consists of a separate vacuum pump connected to an airtight condenser and attached product chamber.

OVERVIEW Freeze drying is the removal of ice or other frozen solvents from a material through the process of sublimation and the removal of bound water molecules through the process of desorption. Freeze drying occurs extremely slowly at these cold product temperatures. Controlled freeze drying keeps the product temperature low enough during the process to avoid changes in the dried product appearance and characteristics.

Product is either pre-loaded into vials which are then transferred to the shelf or it is loaded in bulk form directly onto a product tray. Performance Qualification No water remains in vials or trays after the appropriate freeze drying cycle is performed.


Because of the lack of control over the rate of heat lyophilize into the product, most manifold dryers are operated conservatively at lower pressures to help keep the product temperature lower. Manifold freeze dryers rely on ambient conditions to provide the heat of sublimation to the product. We offer these with Rigid and Bendable probes.

Organic solvents are also removed during primary drying.

When the vacuum level set point is deeper than the vapor pressure of ice at the current product temperature, sublimation can take place. This critical temperature determines the maximum temperature that the product can withstand during primary drying without it melting or collapsing. Typically, stoppering is done on vials with partially inserted stoppers.

The Pirani gauge, however, will give a false high reading in the presence of water vapor.


The condenser temperature required is dictated by the freezing point and collapse temperature of the product. Validation equipment recommended for Autoclaves, Sterilizers and ovens.

SP Scientific service professionals offer your organization a depth of expertise that is truly unique to our selected industries and markets. Understanding the physical properties of materials that are freeze-dried is a key part in developing a successful lyophilization process. The chamber is supplied with clean qualidication for sterilization.

Shelf temperature accuracy and uniformity testing. The tray is loaded with vials, placed on a shelf in the freeze dryer and then the bottom part of the tray is slid out. Each manufacturing facility is an ISO When working with products with low collapse temperatures, it may be necessary to wrap or insulate the flask to slow down the rate of heat transfer and avoid collapse. A piece of aluminum foil can be hung in front of the product on the inside of a pilot freeze dryer as a shield — of course this will block the view of the product and not allow observation during the process.

This website uses cookies to improve your experience. With manifold freeze drying, the process is driven by the system pressure set point and the ambient temperature in the room. Choosing a control system for the freeze dryer depends on the application and use i. Option to use your own thermocouples, or purchase thermocouples ready to go from Ellab. Hydrocarbon levels on swabs should not exceed the negative control. Headquartered in Warminster, Pennsylvania, SP Industries has production facilities in the USA and Europe and offers a world-wide sales and service network with full product support including training and technical assistance.

Additional primary drying endpoint determination tools are available on larger freeze dryers equipped with advanced process control systems. Using the vapor pressure of ice table is a scientific way to determine an appropriate pressure for freeze drying.

Hydrocarbon And Silicone Contamination Silicone levels on swabs should not exceed the negative control. When sublimation of ice crystals is complete, the product temperature will increase and approach the shelf temperature. In addition to defrosting the condenser and cleaning the system after each cycle, routine freeze dryer maintenance typically includes periodic changing of vacuum pump oil and visually checking all seals and gaskets. Similarity in heat transfer characteristics and shelf temperature uniformity is important to ensure that a lyophilization process developed in the lab can be successfully transferred to a production freeze dryer.


Vacuum is maintained in vials. Lhophilizer use of organic solvents requires more attention in the freeze drying process. Purified Water System OQ. Our people make the difference. Sublimation is when a solid ice changes directly to a vapor without first going through a liquid water phase. Annealing has the added advantage of larger crystal growth and corresponding shorter drying times. About Our Trusted Brands.

Basic Principles of Freeze Drying

lyyophilizer Product trays with removable-bottoms are available when working with vials. It is important to allow a modest amount of additional drying time 30 min to 2 hrs, depending on the product characteristics after the product thermocouple temperature increases to ensure that all of the ice in the entire batch of product has been completely sublimated.

The sublimated ice accumulates in the pyophilizer and is manually lyophilize at the end of the freeze drying cycle llyophilizer step. It is not recommended to arbitrarily and repetitively increase the shelf temperature during primary drying, as is seen on some older legacy cycles. Wireless Data Logger Accessories:. The product temperature is monitored using thermocouples and then the shelf temperature set point is slowly increased until the product reaches its target temperature. Also, the flask might break due to uneven stress.

Silicone levels on swabs in the chamber should not exceed the negative control. If renting Rigid units, then the verification application note applies. This valve can be closed for a short period of time and the subsequent rise in pressure in the product chamber can be measured. Sublimation in the freeze drying process can be described simply as: