Advanced Characterization of Solid State Materials

Date: Wednesday, 17 June 2020

Time: 14:00 – 16:00 (CEST)

Venue: Online

The workshop will cover the principles and in-depth study of Dynamic Vapor Sorption (DVS) and Inverse Gas Chromatography (iGC) methods. The presenters will discuss both basic and advanced applications using these methods on studies of solid state materials such as: powders, nanomaterials, and polymers among others.

Both DVS and iGC-SEA are used for research and development in thousands of laboratories in many universities and industries worldwide. This is a good opportunity to learn more about these methods and also ask questions to leading scientists within the field.

The workshop will benefit individuals whose work are in the industry of:

• Biotechnology
• Pharmaceutical
• Biopharmaceutical

Presentation topics:

DVS: Analysis in Drug Development – From Intrinsic Properties to Solid Form Control | by Dr. Jürgen Thun

Developing a sound solid form control strategy is one key task to be performed in the solid state sciences department at Roche during early and late stage pharmaceutical development. Therein, DVS analysis and DVS-Raman coupling experiments support the identification of transformation pathways of different solid forms like polymorphs, solvates, hydrates, salts and/or cocrystals next to other solid state analytical techniques like DSC, TGA, spectroscopy and X-ray powder diffraction. Case studies of complex solid form landscapes highlight the importance of DVS analysis. In addition, determination of the specific surface area using DVS on small sample amounts of Melanin samples was tested. As Melanin can have different synthetic and natural sources, it is interesting to find characterization methods that describe the properties of the material. One natural material is extracted from pig eyes and therefore it is impossible to yield several grams that can be analyzed by traditional techniques. In a collaboration with the Pharmaceutical Profiling department we could demonstrate the power of DVS analysis for such an interesting case determining robustly the specific surface area with around 30 mg of sample.

Surface Area and Surface Energy Studies on Pharmaceutical Powders | by Professor Daryl Williams

The past 20 years particle engineering in the pharmaceutical industry has become a topic of increasing importance especially as engineers and pharmacists seek to understand and control a range of key unit manufacturing operations such as milling, granulation, crystallisation, powder mixing and dry powder inhaled drugs. It has now become very clear that in many of these particle processing operations, the surface energy and the surface area of the starting, intermediate or final products is a key factor in understanding the processing operation and or the final product performance. This paper will consider:

• Surface energy and surface energy heterogeneity of crystalline solids
• Effects of milling on powder surface energy
• Crystal habits and surface energy
• Surface energy and powder granulation processes
• Surface area of low surface area pharmaceutical powders
• Effect of humidity on the surface area of excipients
• And the use of Inverse Gas Chromatography (IGC) for measuring these properties.

Dynamic Vapour Sorption (DVS) Application for the Study of Amorphous Content and BET Surface Area
| by Dr. Damiano Cattaneo

Moisture and organic solvent sorption has a large impact on the mechanical, physical and chemical properties of many materials. This presentation highlights a series of water and organic solvent sorption characterization methods for determining the vapour sorption and amorphous content of different materials. During this presentation we are going to highlight two different methods that can be used to evaluate the ratio of the amorphous content of a material. Moreover, we are going to describe a simple procedure that can be used to measure BET surface area on a variety of samples using the DVS technology. Using a novel dynamic flow configuration, this gravimetric experimental system can measure both competitive multicomponent adsorption as well as water sorption and glass transition processes. This characterization technique can not only be used across a wide range of materials at different temperatures, but is well suited for adsorption studies using organic vapours at high partial pressures.

The presentation will be focused on:

• An introduction to the dynamic vapour sorption, with reference to the historical development of the methodology
• DVS principle and the standard method of data collection
• A description of different methodologies that can be used to calculate amorphous content
• A focused analysis on the theoretical and practical measurement of BET surface area
• The technology that allows the DVS to perform this type of measurement (Speed of Sound sensor)

Panel Discussion – an opportunity for participants to ask questions to the speakers regarding the topics.

Guest Speakers: