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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Processing and formulation development are important steps often taken to make a product ready for freeze drying and usable for its specific application.

Basic Principles of Freeze Drying

This freezing method maximizes the product surface area and minimizes its thickness. This procedure must be run after a lyophilization cycle. Annealing has lyopbilizer added advantage of larger crystal growth and corresponding shorter drying times. A complete thermocouple kit could include the following: All three methods of heat transfer – conduction, convection and radiation, must be considered when freeze drying a product.

One such method entails comparison qualiflcation parallel pressure readings between a Pirani gauge and a capacitance manometer. A suitable container system must be chosen for the product.

When the Pirani pressure reading decreases and approaches the true pressure reading of the capacitance manometer, little or no water vapor is present and it can be concluded that primary drying is complete. Choosing a freeze dryer depends on the product characteristics as well as many other application-based variables including the container that the product will be dried in, the shelf area or number of ports required to accommodate the quantity to be dried in each batch, the total volume of ice to be condensed and whether there are any organic solvents.

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The purpose of the condenser is to attract the vapors being sublimed off of the product. Our unit works with passing the thermocouple straight through the rubber compression materials.

Empty Chamber Temperature Mapping: About Our Trusted Brands. A capacitance manometer always gives a true pressure reading in the product chamber.

When sublimation of ice crystals is complete, the product temperature will increase and approach the shelf temperature. Clamps, Gaskets and port caps are also available.

Condenser cooling rates are for information only.


Additional primary drying endpoint determination tools are available on larger freeze dryers equipped with advanced process control systems. Certain products with high resistance to vapor flow in the dried portion of the cake may require that the shelf temperature be reduced towards the end of primary drying to keep the product temperature at its target and to avoid collapse. It is extremely important that the sample be fully and completely frozen prior to pulling a vacuum and starting the drying process.

Do not include the drain in the average temperature calculation. Shelf temperature accuracy and uniformity testing. Another tool is available with freeze dryer designs that have external condensers. OVERVIEW Qualificayion drying is the removal of ice or other frozen solvents from a material through the process of sublimation and the removal of bound water qualiification through the process of desorption.

Sublimation is a phase change and heat energy must be added to the frozen product for it to occur. Purified Water System IQ. 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.

Find a Product Specialist Request a Quote. Choosing a control system for the freeze dryer depends on the application and use i. Each specific product or formulation that is lyophilized requires the development of a freeze drying process that is based on the unique characteristics of the product, the amount of product and the container used.


Several analytical methods are available for determining that primary drying is complete. Purified Water System PQ. Standard Y fitting with extra port to allow 2 feedthroughs and 1 pressure sensor connected. Determination of the critical collapse temperature of a product is an important step in establishing and optimizing a freeze drying process.

Also, the flask might break due to uneven stress. Performance Qualification No water lyophilizee in vials or trays after the appropriate lyophilizrr drying cycle is performed.

U.S. Valdiation Services – Lyophilizer

Shelf freeze dryers allow the precise control of cooling rates which affects product freezing rates and crystal size. Purified Water System OQ. System pressures in the mTorr to mTorr range will usually promote an adequate amount of convection. Shell bath freezing involves rotating a flask containing the sample in a freezing bath so the sample freezes on the walls of the flask.

System vacuum may be continued at the same level used during primary drying; lower vacuum levels will not improve secondary drying times. This can be accomplished manually using product thermocouples or, if drying in vials, an automated SMART system can be used. Slower shelf cooling rates do not necessarily yield larger ice crystals because of the effects of super-cooling.