Coupling an infrared (IR) camera to a freeze dryer for on-line monitoring of freeze-drying cycles is described for the first time. Normally, product temperature is measured using a few invasive Pt-100 probes, resulting in poor spatial resolution. To overcome this, an IR camera was placed on a process-scale freeze dryer. Imaging took place every 120 s through a Germanium window comprising 30,000 measurement points obtained contact-free from -40 °C to 25 °C. Results are presented for an empty system, bulk drying of cheese slurry, and drying of 1 mL human serum in 150 vials. During freezing of the empty system, differences of more than 5 °C were measured on the shelf. Adding a tray to the empty system, a difference of more than 8 °C was observed. These temperature differences probably cause different ice structures affecting the drying speed during sublimation. A temperature difference of maximum 13 °C was observed in bulk mode during sublimation. When drying in vials, differences of more than 10 °C were observed. Gradually, the large temperature differences disappeared during secondary drying and products were transformed into uniformly dry cakes. The experimental data show that the IR camera is a highly versatile on-line monitoring tool for different kinds of freeze-drying processes.
Keywords: freeze-drying; human serum; infrared camera; infrared spetcroscopy; lyophilization; processing; spatial resolution; thermography; water in solids.
© 2014 European Union.